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Method for Small-Scale Production of Deuterochloroform.

Tansukawat, Natha D; See, Alyaa E; Jiranuntarat, Sadudee; Corbin, Joshua R; Schomaker, Jennifer M.
J Org Chem; 83(15): 8739-8742, 2018 08 03.
Artigo em Inglês | MEDLINE | ID: mdl-29864274
Deuterochloroform (CDCl3) is a common deuterated solvent for nuclear magnetic resonance (NMR) analyses. The synthesis of significant amounts of CDCl3 for both research use and large undergraduate organic laboratories in a safe and inexpensive manner is appealing. Herein, we describe a convenient laboratory scale preparation of CDCl3 that employs a reduction and decarboxylation of hexachloro-2-propanone (HCP) catalyzed by various pyridines. A PVP catalyst gives cleaner reaction and greater catalyst stability through multiple rounds of recycling, justifying its higher cost compared to pyridine.