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Author: Subject: Clomethiazole by Vitamine b1 cleavage
Farbwerke
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[*] posted on 28-6-2020 at 13:25
Clomethiazole by Vitamine b1 cleavage


Fellow campaigners,

Have any of you ever made clomethiazole?  Specifically by means of two reports from the 1930s by:
Studies of Crystalline Vitamin B1. XIV. Sulfite Cleavage. IV. The Thiazole Half
BY EDWIN R. BUCHMAN

I would be interested in the following points:


1.)  The author reports that he extracts the cleavage product with chloroform.  Would dichloromethane also be a suitable alternative?

2.)  Do toxic by-products arise during the conversion of the thiamine cleavage product by means of concentrated HCL.

3.)  Has anyone of you been able to apply the described procedure according to E. Buchman successfully?


Thank you in advance!
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karlos³
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[*] posted on 28-6-2020 at 13:27


Yes the pyrimidine byproduct is very neurotoxic.
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DavidJR
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[*] posted on 28-6-2020 at 16:40


The referenced reports:
https://sci-hub.tw/10.1021/ja01306a044 and https://pubs.acs.org/doi/10.1021/ja01300a086

1. probably, but you would have to try it to find out.
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AvBaeyer
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[*] posted on 28-6-2020 at 20:16


I can say that the sulfite cleavage works quite well. The extraction of the thiazole portion is difficult (tedious) as it requires many extractions. I did use DCM and not chloroform for the extraction. A continuous extraction apparatus would be best but I do not have one.

AvB
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karlos³
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[*] posted on 29-6-2020 at 03:21


This thread might be of interest too: http://www.sciencemadness.org/talk/viewthread.php?tid=154878
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