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Toluene > Benzaldehyde?
Fri Feb 11, 2005 12:39 am |
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quantum
(Hive Bee)
06-28-04 20:41
No 516150
nasty chlorine gass yucky
try hypochorite in toluene use a water bath as if it goes over 105 C it blows. then use a sommelett dont use acetic acid as ethanol is heaps cheaper and works just well trust me I do it all the time now even tried the MnO2 this is the best way as far as I can see I can make about 100G of benzaldehyde from toluene in one day.
jemma_jamerson
(Hive Addict)
06-28-04 22:11
No 516181
orgy
Is this 2nd piece of info accurate?
NO.
would that be temperatures yeild or general procedure mate? or do you mean not practical as in there are other methods covered that are better?
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quantum
(Hive Bee)
06-28-04 23:02
No 516191
Re:just works
na tried nearly every way to aldehyde I could and found this
to work every single time with no problem.
the chloride is pritty nasty I also found that you dont have to distill the chloride just boil off excess toluene
then do the somolett. once somellet is compleate sep with
a bit of water to get rid of ethanols solvent properties
then put the aldehyde in a flask with water and steam distill
no vacume can be done with very little glass I sware it works every fucking time.
ps rhodium you can make benzene from benzoic acid and calcium oxide I did it last night.
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ambi
(Stranger)
07-06-04 02:11
No 517721
Re:someeelot?
Any chance of having quantum's cipher translated into english, or am i missing something here,.?
The toluene to benzal chloride bit is fine, just his proceedure on making the crude benzal chloride into the aldehyde seems sketchy,.
If you are there quantum, please could you elaborate,.
What OTC goodies will convert Benzal chloride into benzaldehyde,.
CaO, Bi-carb,???
ambi
Rhodium
(Chief Bee)
07-06-04 03:18
No 517731
Sommelet: Benzyl Halides to Benzaldehydes
He is referring to the Sommelet Reaction, read more about the mechanism in this thread: Post 495772 (Daphuk_up: "Sommelet vs. Delepine", Newbee Forum)
An example of that reaction being used to turn benzyl chlorides to benzaldehydes can be found in Post 276019 (psychokitty: "Re: piperonyl chloride ---> piperonal", Chemistry Discourse)
The Hive - Clandestine Chemists Without Borders
quantum
(Hive Bee)
07-12-04 22:44
No 519039
sorry been real bizzy
I think it goes 78g of benzyl chloride 168g of hexamine
300ml of ethanol 100ml of water boil for 2 hours the use
200ml of HCl to turn any left over amines into water soluble
salts reflux this mix for 15 min then sep with water and toulene. make sure your benzyl choride is filtered as
any left over hypo could explode.
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Organikum
(Wonderful Personality)
07-13-04 00:02
No 519043
Better method for the Sommelet
"Method of production of aromatic aldehydes by the Sommelet reaction"
BASF AG, Germany
Patent US4321412, in german: Patent DE2942894
The disclosed method avoids the need for alcohol and uses a molar ratio of chlorinated compound to hexamine of 1/1 to 1/1,5.
The patent describes the whole process from chlorination to the final product benzaldehyde.
Using 160gram hexamine for 120gram benzylchloride was tried and works fine. The hexamine can be added directly to the result of the chlorination if chlorine-gas is used. If hypochlorite is used this doesnt work, the reaction product has to be filtered or distilled then, whats a mess and unhealthy. If the chlorination is done with Cl2 it is advantageous to add 0,1% hexamine to the toluene at start - this suppresses ringchlorination.
Remark: Dont try the Loomis method (hypochlorite/toluene) for producing benzalchloride or even benzotrichloride! It works well for benzylchloride though.
ORG |
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