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Author: Subject: Setting up organic chemistry lab - organic experiments
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[*] posted on 18-7-2012 at 11:52
Setting up organic chemistry lab - organic experiments


I am becoming interested in organic chemistry more and more, so I am setting a lab. Those are compounds I currently have:

Organic chemicals:
Urea
Benzoic acid
Citric acid
Acetic acid 9%
Ethyl Acetate
Methyl Ethyl Ketone
Isopropanol mixed with Ethanol
Saccharose

Salts:
Copper (II) Acetate
Copper (II) Sulfate
Potassium metabisulfite
Sodium Benzoate
Calcium Acetate
Calcium Hydroxide
Sodium Chloride
Manganese Dioxide
Zinc Carbonate
Sodium Bicarbonate
Sodium Sulphate

Elements:
Lead
Copper
Zinc
Sulfur
Iron
Silver

Inorganic acids:
Hydrochloric acid 20%

Solutions:
Sodium hypochlorite 5%

Other:
pine resin (maybe something can be isolated?)


Now I don't have means of obtaining sulfuric acid, hydrides and other organic chemicals. I also could get toulene, xylene and some other solvents. I also don't have distillation equipment.

What are some experiments that I could perform, maybe synthesize organic intermediates?

I am thinking acetamide from ammonia and ethyl acetate.
Methylamine from acetamide.
Try to make citrazinic acid from citric and urea.
Benzamide from benzoic acid and urea.

This should be a good start. Anyone know where I could head from here? I am interested in smelly and aroma chemicals.
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zoombafu
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[*] posted on 18-7-2012 at 12:01


If you haven't already download Vogel's Practical Organic Chemistry book from the library. Look through it and find some interesting compounds to make with with you have. (This is how I started organic chemistry)

Ethyl Acetate is fun and easy to make

[Edited on 18-7-2012 by zoombafu]




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[*] posted on 18-7-2012 at 14:07


Quote: Originally posted by zoombafu  
If you haven't already download Vogel's Practical Organic Chemistry book from the library. Look through it and find some interesting compounds to make with with you have. (This is how I started organic chemistry)

Ethyl Acetate is fun and easy to make

[Edited on 18-7-2012 by zoombafu]


Thanks, I will check the book. I would be making esters, but I have no means of obtaining sulfuric acid. Closest I can do is to make dillute 10% by electrolysis.
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[*] posted on 18-7-2012 at 14:54


Go to the hardware store. You can usually find sulfuric acid as drain cleaner.



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[*] posted on 18-7-2012 at 15:39


Just outta curiosity, why not buy some more chems online?
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[*] posted on 19-7-2012 at 00:26


panadol can be converted to hydroquinone and benzoquinone, and supposedly if you have enough reagents and/or are into psychedelics, 2C-B

hydrazine can be made from urea and hypochlorite via hoffmann rearangement

benzene can be had from benzoic acid and a hydroxide

acetone dicarboxylic acid can be had from citric acid

dry distillation of calcium acetate yields acetone in poor yields

aspirin forms salicylic acid upon addition of strong acid

sodium chloride may be electrolysed for sodium chlorate

acid and hypochlorite/MnO2 forms chlorine gas, when bubbled through liquid sulfur makes SCl2

SCl2 and SO3 (dont suppose you have any?) form SOCl2

SOCl2 and a carboxylic acid form an acid chloride

an acid chloride and an alcohol form an ester

potassium metabisulfite and copper sulfate form a copper complex which contains different valencies for the copper ions

IMHO, you really need to get alot more organic chems if you want to do lots of things

if you think you would like to make some modafinil for a studying aid or something, you can start from benzoic acid and go through a long synth to the target molecule, the synth calls for CHLOROacetamide, which can be made from methyl chloroacetate and ammonia

another fun thing to do is take bromoxynil octanoate (which can be found in some pesticides, labeled on the side) and convert it to octanoic acid, octanol etc. for some unique esters

piperonal may be extracted from pepper

capsaicin from chilles (careful!)

sodium bisulfate (from pool shop, pH lowerer) forms sodium (m)ethylsulfate upon addition of the correct alcohol and correct conditions

nitro(m)ethane forms from NaNO2 and sodium (m)ethylsulfate

zinc/iron powder and acid is a strong reducing agent

i believe ammonia can be evolved from urea under certain conditions

silver/copper mesh/wire heated to red heat (900C+) converts ammonia gas to NOx

without sulfuric acid, ester formation looks pretty hard for you, and esters are the nicest smelling compounds IMO

that is all i could think of atm


hope i helped a little:)

[Edited on 19-7-2012 by Lithium]




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[*] posted on 19-7-2012 at 13:37


There is only available HCl for me in my country, no sulfuric acid anywhere. NaOH isn/t available either, I make one by myself with Ca(OH)2.
I don/t really feel like buying chems online either, because I could run into some problems with my country (also most are very very expensive, like 10$ for 100grams of CuO).



Thanks a very nice list Lithium, it will definitely help me with ideas. Im thinking about making SCl2 generator, I just need to find the right materials. From it I could probably make some reactive intermediates.

It's sad that the mustard gas, chloroacetone tear gas, drugs, even nerve agents could be made more easily at home than interesting flavor components. I am not interested in any of those though.

There is odor index in this link:

http://www.thegoodscentscompany.com/index.html

Interesting when looking for flavor compounds.

[Edited on 19-7-2012 by Random]
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[*] posted on 19-7-2012 at 13:47


Copper sulphate can be used to make quite pure conc. H2SO4.

[Edited on 19-7-2012 by plante1999]




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[*] posted on 19-7-2012 at 14:17


Quote: Originally posted by plante1999  
Copper sulphate can be used to make quite pure conc. H2SO4.

[Edited on 19-7-2012 by plante1999]


By electrolysis I could obtain like 10%, but then I am very scared of hot fuming concentrated H2SO4. I don't have glassware either that could withstand those temperatures except test tubes.
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[*] posted on 19-7-2012 at 14:22


Borsillicate glass beaker is made for this purpose. And Conc. H2SO4 is safer than 30% HCl in my opinion.



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[*] posted on 19-7-2012 at 14:27


Well, I'll try to make small amounts first. I could even make catalytic amounts of H2SO4 in the test tube anyway and then proceed to make the ester.

I have forgot how small amount is actually required.

[Edited on 19-7-2012 by Random]
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[*] posted on 19-7-2012 at 15:01


Lithium, whats the synthesis for modafinil from benzoic? It seems I have some starting materials.
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[*] posted on 19-7-2012 at 15:07


google is wonderful!!!

http://www.erowid.org/archive/rhodium/chemistry/adrafinil.mo...




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[*] posted on 21-7-2012 at 21:36


sodium benzoate + NaOH ---) benzene + Na2CO3

6NaBr + 3H2O + 6e- ---) NaBrO3 + 5NaBr + 3H2

5NaBr + 6NaHSO4 + NaBrO3 ---) 6Na2SO4 + 3H2O + 3Br2

benzene + Br2 ---) bromobenzene + HBr

toluene + oxidant (see toluene ---> benzaldehyde thread) ---) benzaldehyde + H2O

Bromobenzene + Mg ---) phenyl magnesium bromide

phenyl magnesium bromide + benzaldehyde --H2O--) diphenylmethanol + Mg(OH)Br

then follow the rest of the synth on rhodium

edit: if you can tell me, what country are you in?

edit2:

acetaldehyde can be made from the oxidation of ethanol

possible ester routes without H2SO4:

http://en.wikipedia.org/wiki/Pinner_reaction

if you set up SCl2 and SO3 generators, you can make lots of SOCl2, which turns carboxylic acids into acid chlorides, which, when added to alcohols, forms an ester

remember; the amount of H2SO4 needed is very small for ester formation, if you decide to make some dilute stuff from CuSO4, boil down until it has a density of 1.3952/ml (50%). store this in a small bottle, and when ester formation is required, add double the amount of acid required to an empty test tube, boil until thick white fumes are emmitted and stopper. the fumes will condense back into sulfuric acid, and the resulting liquid is conc. enough for ester formation, just carry on with the reaction from there. remember yields will be lower than using 98% acid, as boiling only expels so much water.



[Edited on 22-7-2012 by Lithium]




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[*] posted on 22-7-2012 at 13:15


Quote: Originally posted by zoombafu  
If you haven't already download Vogel's Practical Organic Chemistry book from the library. Look through it and find some interesting compounds to make with with you have. (This is how I started organic chemistry)

Ethyl Acetate is fun and easy to make

[Edited on 18-7-2012 by zoombafu]


Is ethyl acetate in Vogel's book? I couldn't find it...
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[*] posted on 22-7-2012 at 14:58


Quote: Originally posted by achem500  


Is ethyl acetate in Vogel's book? I couldn't find it...


Use the index. Page 383.




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