Sciencemadness Discussion Board

I'm setting up an organic chemistry lab...

Lambda-Eyde - 21-6-2009 at 16:51

Gentlemen,


Let me first tell you a bit about myself. I'm from Norway, and I'm sixteen years old. I hope you are willing to see past my age and treat me like any other board member.
Although I know much more about chemistry than other people at my age, I see that the level here is much higher! :o
I'm currently in the Norwegian equivalent of high school, and in August I'll start my second year. I will then study chemistry, physics, molecular biology and mathematics.

I fell in love with chemistry and bought my first pieces of glassware when I was about 10 years old. My interest started in chemistry, then moved on to pyrotechnics. Now I have moved back to pure chemistry, and the pyrotechnics/explosives focused forums I used to eagerly follow didn't really fit my style. ScienceMadness was just what I needed. :)


I believe I am well equipped when it comes to apparatus. I have a 24/40 labset, beakers of various sizes, and flasks of different designs. I'm awaiting a huge shipment of even more apparatus soon, including graduated cylinders, volumetric flasks and a 500g/0,1g balance.

The reason I'm making this thread is because I'd like some advice about chemicals.
I really don't have much chemicals. I do have hydrochloric acid, ammonia, acetone, xylene, potassium and ammonium nitrate, sulfur, sodium benzoate, iodine, potassium permanganate, sodium hydroxide and hydrogen peroxide among others. Most are industrial/fertilizer grade.

I will now present a list of chemicals I will (hopefully) acquire soon:



What am I missing? What does a classical organic chemistry lab have that's not on my list?

Benzene? I will synthesize that myself.
Bromine? Yup.

You may be wondering what sort of reactions am I into? Well, to be honest, I don't really know. Otherwise I would probably not be making this topic.
Oxidize this, reduce that...
As mentioned above, I'd love to make my own benzene. Then I could perhaps nitrate it and make aniline.
Maybe I should brominate it and try my hands at a Grignard? Perhaps too hard for a beginner... :P



So, my bottom line question is; what chemicals are really essential for the average organic chemistry lab? Someday I want to look up a synthesis in Vogel's, and then return to the lab and perform it, because I already have the chemicals.


Puh.. That was a long post. I hope this thread will benefit others as well as myself. Thanks in advance for the answers! :)

Magpie - 21-6-2009 at 17:55

I think you are off to an excellent start.

I recommend that you make a list of the top ten experiments or syntheses that you want to perform. These can come from this forum or other sources, say organic lab manuals. Then prioitize them. Looking at the reagents and precursors required for these experiments will give you your shopping list.

DJF90 - 21-6-2009 at 17:59

There is a plethora of organic reagents and which one to use often depends on the chemo-, regio- and stereoselectivity required. I think your question is too vague though; are you after a list of reagents, or a general list of chemicals that will find use in your organic lab (substrates/solvents/reagents - all these come under chemicals)?

Some reagents that immediately come to mind that you will find most useful:
>Thionyl chloride - allows formation of alkyl and acyl chlorides, and in the case of the former the stereospecificity can be altered by using pyridine.

>TEMPO - Klute has kindly documented his synthesis of this catalytic oxidant (although a complete conclusion was never made...), and it is incrediably useful. Besides being chemoselective (selectivity can be altered by varying they amount of secondary oxidant used), the reaction runs at low temp typically in DCM and produces very good yields in most cases.

>Aluminium isopropoxide - This is especially useful if borohydrides are unavailable, and will allow you to reduce aldhydes and ketones back to the parent alcohol using the Meerwein Pondorf Verley reaction. Works with IPA.

>Diethylether/THF - Indispensible solvents for grignard reactions. I suggest if you don't know these reactions already that you learn them, as they provide a fairly simple method of performing useful synthetic transformations. You'll also want some magnesium granules. Diethyl ether can also be used extensively in solvent extraction as it is a good general solvent for a lot of compounds and immiscible with water.

>Hydrazine or zinc - Useful for removing carbonyl groups using the wolff kishner or clemmensen reductions respectively. Depending on the substrate one will likely be more suited than the other. Hydrazine has the added benefit of being used to make other compounds (interesting ones are luminol and 2,4DNPH), whereas zinc can be used with acid to reduce nitro functional groups (possibly others too). The hydrazine is fine as a salt (eg. hydrazine sulfate).

I'm not going to go on any more, but you will want at LEAST one way to introduce each of the common functional groups. Its good to have more than one method because what is suitable for one substrate may not be suitable for another.

JohnWW - 21-6-2009 at 18:33

Oh, to complete the list you would need, by way of apparatus, a distillation apparatus and associated fittings, thermometers, a pressure gauge, single-necked and three-necked round-bottomed flasks with glass adapters and a muffle-heater and oil-bath heater, pipettes and burettes and a pipette-filler, measuring cylinders (glass and plastic) of various sizes, bunsen burners with gas bottles and gas piping, tripods and metal gauze plates, stands and clamps, glass and plastic and rubber tubing, rubber bungs, conical flasks, a Büchner filter funnel and filter papers with a mains-water-powered conical vacuum flask (or better still a vacuum line powered by a vacuum pump), nickel tongs and spatulas, a fume cupboard with vent, refrigerator for volatile chemicals, safety goggles, rubber gloves and other protective clothing, a water deionizer or distiller, water squirt flasks, glass/rubber "policemen", bumping chips, mortars-and-pestles, a vacuum bell-jar and silica-gel dessicator packs, a drying oven (a pie-warmer will do), magnetic stirrer, analytical/gravimetric balances of various capacities and sensitivities, isolating transformer or RCD to rum appliances from, a basin with waste outlets and taps (including lab taps to fit rubber tubing to), a flask-shaker, a centrifuge, an autoclave (for microbiological work - a pressure-cooker may do for small items), large glass or perspex tanks and glass plates for paper- and thin-layer chromatography, BCF or CO2 fire-extinguishers; and if your budget allows, scanning IR and UV/visible spectrometers, NMR spectrometer, gas-liquid chromatograph.

For additional reagents and solvents besides those mentioned: LiAlH4, NaBH4, anhydrous AlCl3, anhydrous FeCl3, Mg powder, Zn powder, Na metal, Li metal, red phosphorus, liquid Br, NaOCl (bleach), bottled gases (acetylene (or generate it from CaC2), ethylene, carbon dioxide, oxygen, nitrogen, argon, chlorine, hydrogen), acetone, diethyl ether, HBr, HI, HF, HIO4, S, Se, reagents for converting carboxylic acids into acid chlorides (either PCl3, PlCl5, POCl3, S2Cl2, SOCl2, AsCl3, SiCl4, SnCl4, or TiCl4), CCl4, CHCl3, CHBr3, CH3Br, CH3I, acetic acid, acetic anhydride, propionic acid, KCN, CS2; and if you can afford them, Ni and Ti and Pd and Pt and other metals in suitable forms for use as electrodes and heterogenous catalysts. I can name others that would be too dangerous for other than a professional lab. For starting substrate organic materials, and some other solvents: benzene, toluene, methyl salicylate, phenol, cresols, chlorobenzene, dichlorobenzene (from mothballs), anisole/anethole and eugenol and isoeugenol and thymol and safrole and the like from plant essential oils (several of which can be bought as flavorants), starch, cellulose (use cotton wool), glucose, fructose, ascorbic acid, oxalic acid furfural, tetrahydrofuran, pyridine, pyran, pyrrole, thiophene, naphthalene (also used in mothballs), quinoline, benzyl alcohol or benzaldehyde, methanol, 95% and absolute ethanol (can be expensive due to the excise tax on it), n-propanol, isopropanol, n-butanol, amyl alcohol, tert-butanol.

Of course, it would all depend, at your age, on how deep your father's pockets are, and whether you have enough room to store and safely deploy all those reagents and apparatus. An ideal situation would probably be a large shed on a farm, some distance from living accommodation.

[Edited on 22-6-09 by JohnWW]

DJF90 - 22-6-2009 at 06:10

JohnWW: You forgot the rotovap!! :P

Lambda-Eyde: I also assume you will be following most reactions with TLC, and so you will need TLC plates and a variety of stains to reveal the component spots. As I am more awake now, I will be generous enough to point out some other useful chemicals to have:

NBS - useful for bromination of allylic positions by a free radical mechanism. Needs a radical initiator (generally dibenzoyl peroxide). Also has many other uses.

Ammonium formate - Used in the leuckart reaction (in excess) to form amines from ketones (and aldehydes).

DMF - Not only is this a greatly useful polar aprotic solvent, it can also be reacted with grignard reagents to form the corresponding aldehyde (after aqueous workup).

Ph3P - A generally useful reagent. Used in the wittig reaction to form alkenes from ketones. Also used in the straudinger reaction, the mitsunobu reaction, and the appel reaction (off the top of my head).

Pd/C - A nice catalyst for reduction of nitro groups. Very clean and high yeilding (compare the mess created by Sn/HCl reduction :P). Can also reduce other groups (eg. alkenes) and does so at a much lower working H2 pressure than Raney nickel (often atmospheric is sufficient).

NaH - Stong, non-nucleophilic base. Also has other uses such as making NaBH4 and NaAlH4 (can be reacted to form LiAlH4).

NaN3 - I'll mention this one despite it being as toxic as cyanide AND explosive, because it is synthetically useful. The azide anion is a very good nucleophile, and the resulting organic azides can be subjected to catalytic hydrogenation or Ph3P (straudinger reaction) to form amines. Can be used in the schmidt reaction (CAUTION (HN3) - probably not good to do this in an amatuer setting, although on small scale in a hood it should be ok...), and in the curtius reaction (rearrangement).

I think all of the reactions I've mentioned (and many many more) can be found here:
http://www.organic-chemistry.org/namedreactions/

[Edited on 22-6-2009 by DJF90]

The_Davster - 22-6-2009 at 07:21

Sodium azide is not explosive under synthesis conditions. The toxicity is of much greater concern than the energetic behavior of sodium azide. Mind you after reactions, the produced organic azides can be explosive especially if on short-chain molecules.

As Magpie said
Quote:

I recommend that you make a list of the top ten experiments or syntheses that you want to perform. These can come from this forum or other sources, say organic lab manuals. Then prioitize them. Looking at the reagents and precursors required for these experiments will give you your shopping list.

this is the best way, you could have 10 different chemists recommend their favorite synthesis reagents, and none would be in duplicate. Get reagents as you need them for specific reactions, and after you have performed many reactions, you will suddenly find you have a fully stocked lab with chemicals you have experience using(and will use again when you apply the same functional group transformations to new substrates). Otherwise you may end up well stocked, but find you don't know where to start, and will likely end up with things you would never use, especially if you just buy everything mentioned in this thread.

That said, one can never have too many different solvents


[Edited on 22-6-09 by The_Davster]

DJF90 - 22-6-2009 at 08:53

Yes that would be a good idea. I just wanted to provide some options that are quite commonly known so that Lambda-eyde has somewhere to start.

entropy51 - 22-6-2009 at 14:37

I think Magpie's suggestion is an excellent one.

I would also suggest that you get Louis Fieser's Experiments in Organic Chemistry from the forum library. Beginning on page 357 is a long list of the important solvents, drying agents and reagents that were common in 1942. There are obviously many extremely useful reagents that were not in use in those days, but if you had a fair number of the chemicals described in Fieser's Chapter III you would have an excellent start.

I know of one group setting up a lab who just ordered all the chemicals in Fieser's list!

The link to Fieser's book is http://www.sciencemadness.org/library/books/Experiments_in_O...

benzylchloride1 - 22-6-2009 at 18:40

Organic synthesis is my favorite area of chemistry and I welcome you into the field. I also became interested in organic chemistry when I was sixteen. I am now 18 and have a fairly complete organic chemistry lab in my basement. Instrumentation can be a problem, I have purchased many analytical instruments, some of them work and some of them do not. Buying them off of Ebay is Russian roulette. You never know if they will work or not. To start, I would recommend an infrared spectrophotometer, this will enable you to identify functional groups on the compounds you have synthesized. I would be wary though, many of the instruments sold on Ebay do not work because the thermocouples have lost their vacuum. I purchased a PE 467 and the instrument has many problems. I would recommend purchasing a Perkin Elmer 1300 series, this was the best dispersive insturment made and has a pyroelectric detector which seldom goes bad. The newer FTIR spectrometers can have many problems and the dessicant has to be frequently changed.

UV-VIS spectrophotometers are useful for inorganic chemistry for characterising coordination complexes and quantitative analysis. Gas and liquid chromatographs are useful for analyzing reaction mixtures, but are expensive to buy and keep running. I have a gas chromatograph that runs and a HPLC that is a work in progress.

I would recommend buying a rotovap, Buchi brand as they are very useful for removing solvents from reaction mixtures. A fume hood is a must for most reactions, this should be your first priority if you plan on conducting work with organics.

Many of the reagents that you will need or want can be synthesized from fairly common chemicals. If you have a hood, I would run the toluene chlorination experiments that Len1 conducted. Benzyl, benzal and benzotrichloride have many uses in synthesis. Benzene is a must have. Acetic anhydride can be produced by the sulfur chloride/ anhydrous sodium acetate method that is described in the organic chemistry forum of Sciencemadness. The older books have the most useful preparation and start from fairly common chemicals. Many interesting synthesis can be found by browsing the forum or typing in a specific chemical of interest in to this site's search engine. Feel free to send me a U2U message if you have further questions.



[Edited on 23-6-2009 by benzylchloride1]

zed - 22-6-2009 at 21:30

Take as many chemistry classes as you can. Ask your professors if you can do some extra credit projects on campus. Without mentoring, the life of a young chemist can be brief. As a bonus, generally speaking, campus chemicals are FREE chemicals.

There is no point in buying things you may never use. I suggest you buy things as required, or in the case of truly difficult to acquire reagents, as opportunity presents itself.

Rather than stocking up on lots of expensive and difficult to handle toxic chemicals....... I suggest that you buy/ or build for yourself.....a reliable fume hood.

With gloves and a good fume hood, most toxic materials can be handled safely, and most projects thereby become possible.



Magpie - 23-6-2009 at 15:53

Good advice, zed.
Quote:

Without mentoring, the life of a young chemist can be brief.


Did you mean this literally, or did you mean "...life as a young chemist can be brief." :o

zed - 26-6-2009 at 02:49

Whichever sounds most ominous.

Personally, I was initially mentored by a Senior Pharmacy Student.

I was pretty green, so I asked him to help me during my first few organic chemistry experiments. That proved to be a good idea.

We were using Diethyl Ether in a marginally ventilated space, without a fume hood.

My mentor pointed out useful little things.......Like our needing to either tape down the light switches, or replace them with explosion proof switches. Otherwise, with the nonchalant flick of a switch, we might be blown to kingdom come.

Probably wouldn't have occurred to me that there was any danger.

So easy to take some lessons, from an experienced hand.

So expensive to have your own hands stitched back on, after a disastrous mishap.







entropy51 - 26-6-2009 at 05:38

Ether vapor is so dense that it usually crawls along the floor, too low for the light switches to set it off. But a good precaution nevertheless.

People often forget about the pilot light on the water heater however...:o

Lambda-Eyde - 7-8-2009 at 19:00

Oops! It's been over a month! It's about time I replied. Thanks to all of you for the helpful, informative answers, it's appreciated!
Quote: Originally posted by Magpie  

I recommend that you make a list of the top ten experiments or syntheses that you want to perform. These can come from this forum or other sources, say organic lab manuals. Then prioitize them. Looking at the reagents and precursors required for these experiments will give you your shopping list.

That sounds like a smart thing to do. I'll do that.
Only problem is, I discover new things I want to do every day! Therefore I'd like to have the common organic lab chemicals already at hand.
I'll speak to you later about my fume hood.


DJF90: Thank you very much for your long answer. Most of the reagents you mention are out of the question, or I don't think they interest me much. I can buy diethyl ether and acetic anhydride fairly easily from Fisher Scientific, I expect I'll be using those two (especially the ether) fairly often.
I'll also have to get some methanol from them...

You mention DNPH (2,4-dinitrophenyl hydrazine). I'd very much like to synthesize that: Benzene -> Chlorobenzene -> 2,4-dinitrochlorobenzene, then react with hydrazine sulfate to form the final product. I can't get hydrazine or any of its derivatives, so I'll guess I'll have to synthesize my own (which sounds like a major pain in the ass). I guess that's the life of a chemist!
You also mention NaBH4. I can get ahold of that easily and fairly cheap, but I don't think I have enough experience to handle such a vicious chemical yet, nor do I have any immediate use for it.

I've been thinking of getting some silica TLC plates, if only they weren't so expensive. Also, I hate "wasting" solvents on stuff like that.
Ammonium formate I believe can be synthesized from ammonia and formic acid? Sounds fairly trivial for such a useful chemical.
I'm thinking of getting some NaH too, it sounds relatively easy to handle compared to the boro- and aluminium hydrides, and not to mention how much cheaper it is. 20$ for 100 grams, that's not too bad, is it?

Pd/C: Unless I get a REALLY good deal, that's not happening! I'd like to make some Raney nickel myself, and perhaps a simple hydrogenation apparatus for relatively low pressures. I'd very much like to explore the field of catalytic hydrogenation!
Oh, and I'll stay away from the azides and cyanides for now! :o


JohnWW: Wow, wow! I'm not on a university budget here! :o
On my shopping list for apparatus only, I have among other things a vigreux column, 250 ml three-neck, 50 ml buret, hotplate stirrer (I'll probably buy one from ebay.de), more 24/40 stoppers (I can't believe a labset with 5 flasks come with one stopper!), larger 24/40 round bottom flasks, a 1L heating mantle, an aspirator, and if I can earn enough cash, a spectrophotometer. Seems like I didn't mention in my original post that I do have a magnetic stirrer.

And a 16-year-old with an NMR spectrometer in his basement? I wish! :D

You mention safrole, why would I need that? The only synthesis I know of which use safrole oil is MDMA/ecstacy. The only thing I'm cooking is food!

Bottled gases are out of the question. I'd love to have a bottle of nitrogen in the lab, but the prices are insane. A friend of mine whom I am building a workshop together with went to a welding supply house and asked about prices on bottled gas (we're getting a MIG welder). The clerk told him we'd most likely end up paying more for one year of bottle rental than the welding machine itself! Really, Yara's monopoly on bottled gas is just ridiculous! So I'll have to stay away from that unless I find a reasonable supplier.

Is there perhaps anyone here familiar with how this works in Sweden? If so, I'd love a U2U. :)
Quote: Originally posted by JohnWW  

Of course, it would all depend, at your age, on how deep your father's pockets are, and whether you have enough room to store and safely deploy all those reagents and apparatus. An ideal situation would probably be a large shed on a farm, some distance from living accommodation.

Mind you - I have a job of my own! ;) My parents haven't paid for even a single erlenmeyer.
My lab will be situated in the basement, and therefore I will avoid storing something incredibly dangerous or doing very risky (read: foolish) experiments. I store all my chemicals in a locked metal cupboard, and when I move into my finished lab I'll hopefully be able to store them even safer - separate oxidizers and reductors, and provide ventilation for the flammable solvents.


entropy51: Thank you. I'll make sure to read that book!


Benzylcloride1: Thank you! :) I look forward to discussing with you later!

Thank you for the advice on spectrophotometers, as I have a fairly limited knowledge about them. I have read a little bit about UV-vis spectrophotometers, and even found one on eBay for ~400$ with freight that I'm considering. However, if I am to believe you, it's not very useful in organic synthesis? That's a shame. The only thing I know about IR spectrophotometers is that they are very useful, but can also be a major pain in the ass, considering all the extra work needed. Dessicants, purging gas, not being able to use normal cuvettes etc.
I will take your advice and read more about IR spectrophotometry and be on the lookout for some on eBay.

I'd love to have a gas chromatograph, but I find the price to be quite prohibitive. Someday..!

A rotavap would indeed be nice, but I seriously doubt I'll get one.

Chlorination of toluene would indeed be interesting, and a fumehood is my second priority right now (after renovating the room where the lab will be). I have read a fair bit of len1's articles, and I must say I'm impressed! Quite inspiring.


zed: What? I said high school, not university! :P There are no professors here, only a single chemistry teacher... Who also kindly donated a 250 ml Electromantle to me! I don't think I can expect much mentoring from him, although I will most certainly confer a lot with him. He's quite a jolly guy, who really endorses my hobby!


Phew, is that all of you? :P

Addendum: Recently I've discovered (Thanks to O3-labs!) that I'd like to explore azo dyes. I guess I'll be making a fair amount of aniline and shopping a dash of sodium nitrite!

smuv - 7-8-2009 at 22:47

A lot of my early organic chemistry experiments revolved around ethanol. From one cheep precursor you can make many compounds which are interesting to make in their own right, but also useful in future endeavors. You don't need a rotovap or fume hood for just starting out, all you need is common sense of chemical toxicities, a distillation setup and for some experiments, the outdoors. Things I have made from ethanol:

Ethylene
Ether
Ethyl nitrite (burns w/ white/grey flame)
Ethyl bromide
Ethyl chloride (burns with blue green flame)
ethyl sulfuric acid

[Edited on 8-8-2009 by smuv]

DJF90 - 8-8-2009 at 00:57

Lambda-Eyde: Sodium borohydride is fairly benign, especially relative to LAH. Just keep it in dry conditions like you would any other chemical and be careful what you mix it with. Its very useful, as you can do several different things to modify its reactivity, and I would say it is a necessity in the organic lab (although there are always alternatives, but generally not as nice...).

The synthesis of 2,4-DNPH and hydrazine will be good experimental procedures and I feel you will learn a fair deal from this.

TLC plates are expensive but are useful for following reactions. I do not feel that it is a waste of solvent - you only need to use a small amount and even so, the solvent is generally cheap (mixture of EtOAc and pet ether is an example solvent system).

Sodium hydride is alot more difficult to handle than NaBH4, although less so than LAH. If I'm not mistaken it can catch fire in a moist atmosphere. It is not a reducing agent like NaBH4 or LAH though (your post seemed to imply you thought it was...), however it is a very good base, which can in some instances be used to double deprotonate substrates to get a different regioselectivity.

I don't blame you for shying away from azides and cyanides, but as you gain experience you will want these chemicals, as they are versatile and very useful in organic synthesis.

You will also want to get some magnesium - grignard reactions are very useful in organic synthesis, and although the procedure can be a little tricky to begin with you'll soon get the hang of it.

Lambda-Eyde - 8-8-2009 at 09:02

smuv: I wish pure ethanol was that easy to get. All technical spirits where I live are contaminated with various ketones and esters, and are useless for anything but cleaning! Seems like I have to get that from Fisher as well.

Btw, looking through Fisher's website I found a product with the following description:
"Ethanol 96% denaturated with 20% propanol-2"

What the heck is that supposed to mean? The percentages don't add up...

Anyways, thanks for the suggestions. I'll make sure to check out most of them.


DJF90: Ah, yes, I always mix up when talking about the hydrides. Anyways, the NaH I was thinking of is sold as a 50% suspension in oil, not as a dry powder.
There's something about extremely reactive and pyrophoric solids that make me shit my pants... :(

Neither EtOAc or petroleum ether is OTC here, therefore I'll have to get those from a lab supplier, too. Which means I'll soon run out of money... The only pure OTC solvents I can get are isopropanol and xylene, as all the others are contaminated with some useless crap.

I understand that I one day will want to acquire some sodium azide, as it is fairly useful. I'll probably make my own cyanides. However, I'll stay away from these reagents and others of similar toxicity (although I could use some phosgene) until I have much more lab experience and feel I can handle them safely.

I have read a lot about the Grignard reaction (it's rather ingenious) and I'd really like to try them out one day. I'll have to get some more experience first before I try my hands at such a difficult reaction. Magnesium is quite useful for other things as well, so I'll probably get some anyways.

ammonium isocyanate - 9-8-2009 at 09:49

I too am just getting my lab up and running, although I have been doing experiments while I work on acquiring equipment/reagents. My lab, however, is intended to be for both organic and inorganic chemistry. Here are some of the things I would recommend:

Solvents:
Glacial acetic acid
Ethanol
Isopropanol
Petroleum ether
Ethyl acetate
Acetone
Kerosene
Toluene
Distilled water
Diethyl ether
Limonene
Hexane
Heptane
Tetrahydrofuran
Methanol
Xylene
Benzene
Chloroform
Dichloromethane
Liquid ammonia
Triethylamine
Nitrobenzene
Pyridine (hard to get, I know)
Carbon tetrachloride (same deal)
Carbon disulfide (more of the same)


Obviously it would be very hard to acquire all of these solvents, particularly the last three. You don't need all of these solvents. Certainly, there are a number of exteriments one can do with just a few. But some rainy day you'll stumble upon some interesting historical paper for the synthesis of compound x by coupling a and b in solvent c, and you'll be sad if you don't have it. Or you'll get some residue on your glassware and be unable to remove it. Or you'll be attempting an extraction and can only seperate out a specific component with a solvent you don't have. Bottom line is, get as many solvents as you can find and store.

Other very useful reagents for organic chemistry:
Sulfuric, Nitric, Hydrochloric, and Phosphoric acids
Sodium nitrite
Sodium azide
Sodium cyanide
Sodium bicarbonate
Sodium and Potassium hydroxides
Sodium and Potassium iodide
Sodium, Lithium, Potassium, Calcium, Aluminium, Magnesium, Zinc, Copper, Silver metal
Silver nitrate
Silver oxide
Copper(II) oxide
Iron(II) sulfate
Aluminum, Iron(III), and Zinc chlorides
Red phosphorus (good luck finding it)
Bromine
Iodine
whatever organic molecules you're trying to manipulate

turd - 9-8-2009 at 22:14

Quote: Originally posted by ammonium isocyanate  

Solvents:
...
Petroleum ether
Kerosene
Hexane
Heptane
...
Benzene
Xylene
Toluene
...
Dichloromethane
Chloroform

Lots of redundancy in there.

Quote: Originally posted by ammonium isocyanate  

Limonene
Nitrobenzene

These are quite unusual solvents.

Quote: Originally posted by ammonium isocyanate  
Red phosphorus (good luck finding it)

OTC in most parts of the world. I can buy a kg of that over the counter without raising the slightest of an eyebrow, though it would be quite (too) expensive. Remember: you are not the centre of the universe. ;)

[Edited on 10-8-2009 by turd]

JohnWW - 10-8-2009 at 00:43

Another two that do not seem to have been mentioned before: S and Se, which are of use in some organic syntheses, and also of use for making organosulfur and organoselenium compounds. For making organometallic compounds, highly reactive inorganic compunds of metals would be needed. Oh, and do not forget the acetic anhydride, important for protecting -OH groups in some organic reactions.

ammonium isocyanate - 10-8-2009 at 07:58

turd:

Having several solvents with similar structures is very useful. For one thing, pet ether is cheaper than hexane or heptane, but not suitable for some sensitive processeses. Thus you use less expensive reagents. Another important thing is bp. The easiest method of temp control is to use a solvent at reflux with a bp at or near the optimal reaction temperature. Benzene boils at 80.1C. Toluene boils at 110.6C. Xylene boils at ~139C. That can make a pretty big difference. And as for DCM versus chloroform, they really do have considerably different solvent properties, as chloroform is non polar whereas dichloromethane is polar aprotic.

Furthermore, as I said I'm not saying one must have all of the solvents I listed. For example, where I live hexane is hard to get, but heptane is OTC.

And you're right about the red phosphorus thing. I'm so use to the US attitude about it that I forgot about its availability abroad. Is it OTC where you live, and if so what is it used for? Or is it just you can buy it from a chem supplier?

Ozonelabs - 10-8-2009 at 08:53

We have all of the solvents you listed, as well as some others ammonium isocyanate, and they most certainly are all used. Solvents aren't very interchangable for some reactions, and as such having a diverse array of options is a very useful tool.

Rich_Insane - 10-8-2009 at 08:58

Be aware that setting up an organic chemistry lab can be excruciatingly expensive. Instead of stocking everything and experimenting right away, you should take some time, look for good sources, then begin stocking up, then start experimenting. At least that's how I'm attempting this. But I'm poor as hell (I'm too young to find a job), so it may be different for you. I can barely afford a few flasks and beakers.

I did find a supplier a bit ago called Daigger (I have a thread on them), they might be a good source for you. Apparently they do ship to private addresses.

I agree with Ammonium. You should stock some industrial hydrocarbon mixtures as well as the pure reagents and solvents. For example. Stock both ACS grade H2SO4 and drain cleaner H2SO4. This way, you can save by not buying 2.5 L of ACS H2SO4, and use the cheaper H2SO4 for times when you want to do something really simple. I would recommend stocking some brominating agents. I'm not sure if I am biased because I learned O Chem with Br as the perfect halogen, but it seems pretty handy to me. I would say HBr for a start, them PBr3 or something. I would definitely invest in a good fume hood, because you could probably continue doing some of the more dangerous reactions inside the fume hood.

Gringards may be a little difficult for a starter, because organometallics can be quite hard to work with. I would do something simple to synthesize alcohols with different alkyl halides (NaOH + alkyl halide) first. Obviously you have a lot more equipment than me, so I'd go ahead and just read up on some cool reactions.

If it seems interesting to you, you could play around with extraction of alkaloids (etc.) from plants.



turd - 10-8-2009 at 10:46

Quote: Originally posted by ammonium isocyanate  

And you're right about the red phosphorus thing. I'm so use to the US attitude about it that I forgot about its availability abroad. Is it OTC where you live, and if so what is it used for? Or is it just you can buy it from a chem supplier?

Some drugstore-like shops also sell plain chemicals. They even order from Merck, although with a hefty surcharge. One I know stocks red phosphorus, but don't ask me what it is good for. Personally, I used it for the classic P(red)/I reduction, for example of mandelic acid.

Everado E. Dinavo - 13-8-2009 at 16:15

Quote: Originally posted by Lambda-Eyde  

...
Btw, looking through Fisher's website I found a product with the following description:
"Ethanol 96% denaturated with 20% propanol-2"

What the heck is that supposed to mean? The percentages don't add up...


I think that means a 20% v/v solution of isopropanol in 96% ethanol. Which is pretty much useless for anything but cleaning. I've always thought it unfair that one of the most useful chemicals in a lab is so hard to get in a pure form.

benzylchloride1 - 16-8-2009 at 20:48

Back to spectrophotometers, IR is extremely useful, but is proving very expensive. I would recommend buying a Perkin Elmer 1310. Parts are still available for this instrument. I recently puchased one off of Ebay. I turned the instrument on and within 5 minutes the detector died! I am in contact with an IR guy on LabX and I will be able to get the replacement detector for several hundred dollars and have a running instrument. The 1310 has a pyroelectric detector which is faily inexpensive to replace; hundreds instead of thousands of dollars. Polyethylene can be used as a window material for IR cells; many disposable IR cards are made of polyethylene cards, use white plastic grocery bags. It will not hold up to heavy duty organic solvents.
I would recommend a Perkin Elmer Lamba 3B UV-Vis specrophotometer if you wish to do any inorganic or quantitative work. This instrument has few problems, except that the deuterium lamp for UV work is extremly expensive. I recently aquired one of these off of Ebay in complete working condition. They require a chart recorder to print out a spectrum. At least chart recorders are dirt cheap off of Ebay. Plan on paying more for the paper then the recorder.
Hydrazine sulfate can be made fairly eaisly by Roscoe Bodine's method. Run the synthesis at half scale using the exact conditions and proportions in the procedure. I was barly able to get away with using a 3 Liter flask due to the amount of foaming. The half scale procedure will give you about 100g of hydrazine sulfate, enough to make plently of 2,4-dinitrophenylhydrazine. The hydrazine sulfate can also be converted to sodium azide by methods that are posted on this forum. Many organic experiments can be conducted with out a fume hood, but shy away from reactions involving chlorine, bromine, lachrymators and higly toxics until you get a hood. It is nice to have both 14/20 and 24/40 glass ware sets. The 24/40 set is useful for making compounds in fairly large quantities. After several steps of a multiple synthesis, you will seldom have a large quantity of product, the 14/20 kit then comes in handy especially for distilling products when you have less then 50mL due to the minimum amount of holdup.


[Edited on 17-8-2009 by benzylchloride1]