Sciencemadness Discussion Board

Any of these chems OTC?

conducter - 4-1-2007 at 06:08

i was recently looking up the synth of Safrole from Catechol and while i thought i was lucky being able to find a source for Aliquat 336 the other chems were hard to find. so i guess im here asking if anyone knows of where to get these chems if they are OTC or swim should just give up..

N-bromosuccinimide

Magnesium turnings

Dibromomethane

Copper (I) iodide

Ally Bromide

OTC

MadHatter - 4-1-2007 at 07:03

Copper Oxide - Find a well-stocked pottery/ceramics shop for it. Magnesium - Walmart stocks
firestarter kits. You'll have to grind up the Mg yourself. Sorry, but I don't know about
the rest of those compounds.

conducter - 4-1-2007 at 07:20

Copper Iodide not oxide. I believe its made with sodium or potassium iodide solution and copper sulfate. And results in Copper iodide and Iodine.

Magnesium isnt a big deal.

I found out Allyl Bromide can be made using Allyl Alcohol which is made with Oxalic Acid and Glycerol.

So now i really only need to know how to get or synth Dibromomethane and N-Bromosuccinimide.

I found a synth for dibromomethane from 88% Bromoform but i cant find out how to get or synth that either.

Sauron - 4-1-2007 at 07:31

Bromoform is easily made by the haloform reaction in analogous manner to chloroform and iodoform.

Look it up in Vogel, Practical Organic Chemistry 3rd Ed. which is available free from forum library.

Bromoform may well be a (DEA) controlled substance depending on where you are. Be warned.

Sauron - 4-1-2007 at 07:35

Also I believe there was a methylene bromide (dibromomethane) prep on Rhodium. You might ask one of the guys who has that archive for it.

conducter - 4-1-2007 at 07:57

yes the one on rhodium is the one i was referring to.

One needs hypochlorite and acetone/alcohol to create Chloroform.

What chems would be needed for a Haloform reaction to get bromoform?

Sauron - 4-1-2007 at 08:11

If you think about that for a moment I'm sure the answer will come to you. In general doing things a la cookbook without knowing why you are doing what you are doing, understanding the reactions and the mechanism, is a path fraught with peril.

The Vogel book does explain all that if you get stuck for an answer on your own.

Also same book has prep of CH3Br2

I think the chapter is called Polyjalogen Compounds.

NBS (N-bromosuccinimide) is easily made from succinimide and bromine. Succinimide is easily made from succinic acid and concentrated NH4OH. Or you can just buy the NBS. You might find bromine hard to get and a hassle to prepare and if you don't have the skills or experience to safely handle a liquid halogen (stinks, burns you, chokes you, bad for your eyes etc.) then it is better to avoid it.

Sauron - 4-1-2007 at 08:33

I hope you understand that I will help you more by not spoonfeeding the answer to you.

You see, you answered your own question, it's right in front of you but you didn't see it yet. Read back what you wrote and let the light bulb over your head start to incandensce. Glow, tunsgten, glow!

Maja - 4-1-2007 at 13:05

N-bromosuccinimide

This one isn't OTC at least in my country, succinimide costs a lot of... And NBS cost a fortune... I suggest you to try making your own starting from succinic acid.... You can find this one for ~40$

Magnesium turnings

I was unable to find any Mg in my country. No one ever heard "fire starters"

Dibromomethane

I knew a few suppliers for DBM for ~30$ for liter ,but in my strange country...

Copper (I) iodide

Can be made. I think that you can replace bromide instead iodide... Bromide is easy to get in my country.

Allyl Bromide

Oxalic Acid + Glycerol ---> Allyl alcohol ,but yields aren't that great... But I hope you need small amounts...

Fleaker - 4-1-2007 at 16:38

No Mg fire starters? That's a shame as they're relatively pure. I suppose you could look for magnesium wheels or magnesium castings of some sort, but they're hardly 'Grignard' grade...

Sauron - 4-1-2007 at 19:09

@conducter, did you sort out the bromoform preparation?

Was Vogel helpful? Vogel has preps for NBS, succinimide, bromoform, and methylene bromide, which is a sybstantial part of your list.

Maybe you know this already and maybe you don't but, you should routinely look for what you want in the website of Organic Syntheses (Http://www.orgsyn.org/) because it is free, searchable, and the preps are clearly written, checked and thoroughly noted and annotated.

turd - 5-1-2007 at 02:45

Quote:
Oxalic Acid + Glycerol ---> Allyl alcohol ,but yields aren't that great... But I hope you need small amounts...

He's obviously trying to make MDMA or MDA, that means with allyl alcohol he's still something like 6 or 7 steps away from his product. Some reactions will have 50% yield or less. Personally, if I would try that, I wouldn't bother with anything below 100g allyl alcohol.

Sauron - 5-1-2007 at 05:42

The hard knocks associated with cumulative losses in long synthetic strategies are part of the learning curve for all of us, aren't they? Yes it is pretty obvious what he hopes to make (eventually) but it is also pretty obvious he's a tyro (and I mean that in the nicest way, we were all tyros once.) Unless he has a real commitment to organic chemistry and is not just chasing a fast buck he is going to burn out before he gets anywhere near the end.

Whether or not he stays the course he may at least learn something along the path. I tried to help him pedagogically. No point in lecturing him about the wisdom (or -un) of his project. Probably would tune us out anyway.

Maya - 5-1-2007 at 07:35

Well that is what separates true hard chemists from the weekend warrior chemist isn't it?

a real one knows pretty much by looking if it'll be feasible to even attempt one route versus another; after all there are seriously a great many number of routes possible to any compound , but only one or a precious few routes that are actually practicable to undertake

Sauron - 5-1-2007 at 13:41

Damned right. Now compound that with the need to start with a Kg or more of starting material in order to end up with (10+ steps later) 25 g of final product; lots of wetlab in between, and the need to work in larger equipment in the early stages (or do same preps many times.) All in a day's work, but comes as a shock to the quick buck artists.

Personally I always have preferred macro and prep scale work, rather than semimicro and micro, a smudge in the bottom of a sample vial just never seemed worth all the effort. A quarter kilo of something nice and pure in an an evaporating dish coming out of a drying oven, is another story. A definite feeling of accomplishment.

Sauron - 5-1-2007 at 14:14

Now I have always been an admirer of the Org.Syn. series. Maybe 6 years ago after a long period in my life when I was essentially cut off from chemistry, I snagged about 151 consecutive annual volumes from Vol.50 through Vol 64 in hardcover and a further decade or so a few years later in the not nearly as nice paperback personal editions.

So I started reading these and before long struck upon the idea of replicating as many of these tried and true procedures as practicable.

To my horror I soon realized that many of these procedures could not be so easily repeated today simply because so many of the necessary reagents or solvents have been banned or restricted. Unless one has a large corporation or institution backing one up, in many cases this simply is a dead end, or at best adds a lot of extra labor. Having to make one's own CCl4 or CHCl3 for exampel. Or ethylene dihalides. Or acetic anhydride. Most of the classical chlorinating reagents. SOCl2, SO2Cl2. PCl3, PCl5, POCl3. Things we used to take for granted. Damn.

Rosco Bodine - 5-1-2007 at 15:13

Quote:
Originally posted by Sauron
Personally I always have preferred macro and prep scale work, rather than semimicro and micro, a smudge in the bottom of a sample vial just never seemed worth all the effort. A quarter kilo of something nice and pure in an an evaporating dish coming out of a drying oven, is another story. A definite feeling of accomplishment.


Hehehe ...I know that perspective :D

Gets to the point where you stop thinking about
pouring and measuring and think about pumping
and flowmetering , strain gauge weighing for
your reaction vessels additions ...... instead :D

It all becomes so very industrial scale as things
get a little out of hand !

I have a couple of old sliding glass doors which I use
for drying trays outdoors in the sun when the weather is favorable . I support each one near the ends on inverted five gallon buckets , and pull a sheet of black plastic flat across the glass and tape the corners to the underside .

Dumping ten pounds of damp crystals of whatever onto
the center of the black poly and spreading it out in a thin layer in the sun , it air dries very well and the black plastic
gradually warms up to actually bake out most residual moisture .

I have six large Erlenmeyer flasks of 6 liter capacity and
a 12 liter Florence , some 1.25" D 4 , 5, and 6 inch stirbars for churning hot solutions as they cool during crystallizations ,
sitting on a Maxi stirrer which has a 1/8 hp blower cooled
drive motor .

I used to have a 16 speed 1/2 hp counter-rotating mixer
but got rid of it because it was really overkill for anything .

I also have a 1.2 meter custom Kontes graham condenser
a hundred loop coil in it I think ....and some other interesting
trinkets collected over about 30 years time .

roamingnome - 5-1-2007 at 15:15

when you cross the line into life passion vs. the "other thing" you really become a good steward of the earth.

for example i wouldnt think to just waste wood ash.... oh no

egg shells .. heck yeah....
even the protein sheath of the egg shells contains hyaluronic acid, but im not batting at that any time soon....

Rosco Bodine - 5-1-2007 at 15:21

You know you are pretty well at the limit of your hobby
when you actually have to figure in the electricity cost
of running all the equipment for your next experiment ....
and may have to spread it out over a couple of months
just so you can pay the damn light bill :D

And funny you should mention wood ash , I have saved about thirty pounds of it , accumulated in a plastic tub .....
just knowing it will be useful for something at some point :D

[Edited on 5-1-2007 by Rosco Bodine]

Iodide

MadHatter - 5-1-2007 at 23:44

Sorry, I should have had my reading glasses while viewing your initial post. I'd look for
potassium iodide at a photographic supply shop. Probably not OTC, but the other use
I can think of, right off hand, is in tablet form for radiation exposure. It should react
with copper sulphate to give you what you want.

Sauron - 6-1-2007 at 00:01

@Roscoe

I have about a dozen Cole Parmer Masterflex peristaltic pumps for precisely the reasons you elaborate. The fun ones are the PTFE heads and the PTFE diaphragm heads. They can pump most anything. Next best iare the more conventional heads using Viton tubing. hey can pump nearly anything. But not as resistant as the PTFE.

When using this sort of stuff we are really mimicking chemical engineering, process chemistry.

In glass there are constant flow pressure equalizing addition funnels with standard taper joints but they get pricey in the large sizes. As in anything else: if you have to ask how much a piece of glassware costs you probably can't afford it.

Most of my really large stuff is left over from my liqueur making days. 72 L rb flask, two 4-necked and two 1-necked. The joints are mostly 45/50 and 55/50 but the center joints are flanged and Kalrez O-ringed for matching heads, and those have very large joints for BIG costly fractionating columns. I have a pair of new never used Glas Col mantles also 72 liter. A tabletop Buchner funnel in PE 30" wide and 12" deep with a medium frit, bought it from a guy who was into commercially recovering Ag from photographic and X-ray lab waste. A 20 liter Buchi industrial Rotavap R-152 with the double descending glassware set and a pair of 10 L receiving flasks. (a lot of $$ tied up in that.)

Don't have the giant columns as the biggest one I have is only a meter or so long, 29 mm ID Hempel silvered and jacketed with bellows. A 50/30 ball joint on bottom and a 29/42 standard taper on top. I have the matching 5 L flask with a thermowell, it was a refluxing hexane still in a university lab, snagged it on LabX for $80 but getting it to Thailand in one piece was a bitch.

Every bit of that was for the absinthe making and when I got out of that I couldn't bear to sell this stuff off. Now it is gathering dust. Maybe someday I will find a use. Most likely is recycling HPLC grade solvents for prep HPLC work.

[Edited on 6-1-2007 by Sauron]

Maja - 6-1-2007 at 03:23

Quote:
Originally posted by conducter
Copper Iodide not oxide. I believe its made with sodium or potassium iodide solution and copper sulfate. And results in Copper iodide and Iodine.


He needs +1 oxidation state. That can be achieved by procedure from Vogel :
Quote:

21. COPPER(1) BROMIDE
Dissolve 45 g (0.18 mol) of copper(rr) sulphate pentahydrate and 19 g (0.19 mol)
of sodium bromide in 150ml of water. Add, with stirring, a solution of 11.8 g of
sodium metabisulphite in 120ml of water to the hot solution during 5 minutes
(1). If the blue colour is not completely discharged, add a little more sodium
metabisulphite. Cool the mixture and decant the supernatant liquor. Wash the
precipitate by decantation with water containing a little dissolved sulphur
dioxide to prevent oxidation. A solution of copperfr) bromide may be prepared
by dissolving the moist solid in 30ml of constant boiling point hydrobromic
acid (48% w/w HBr). If however the solid salt is required collect the precipitate
in a Buchner funnel, wash with water containing a little dissolved sulphur
dioxide, followed by ethanol and then ether each containing sulphur dioxide and
press with a glass stopper. Remove residual solvent and finally dry the solid in a
vacuum desiccator over sulphuric acid and potassium hydroxide.
Note. (1) Alternatively pass a stream of sulphur dioxide through the heated solution
(60 "C) for about 2 hours.
An alternative means of preparation of a solution of copperfr) bromide
involves heating under reflux a mixture of 63 g (0.25 mol) of copperfrr) sulphate
pentahydrate, 20g (0.314mol) of copper turnings, 114g (1.109 mol) of sodium
bromide, 30g (16.3 ml) of concentrated sulphuric acid and 1 litre of water for 3-4
hours. If the colour of the solution has not become yellowish after this period of
heating, a few grams of sodium sulphite should be added to complete the
reduction.

unionised - 6-1-2007 at 08:27

True, but it can also be obtained by the simple reaction of copper sulphate and potassium iodide. Iodide is able to reduce copper(II) to Copper(I).