Method for Small-Scale Production of Deuterochloroform

被引:4
作者
Tansukawat, Natha D. [1 ]
See, Alyaa E. [1 ]
Jiranuntarat, Sadudee [1 ]
Corbin, Joshua R. [1 ]
Schomaker, Jennifer M. [1 ]
机构
[1] Univ Wisconsin, Dept Chem, 1101 Univ Ave, Madison, WI 53706 USA
基金
美国国家卫生研究院; 美国国家科学基金会;
关键词
CHLOROFORM-D;
D O I
10.1021/acs.joc.8b01018
中图分类号
O62 [有机化学];
学科分类号
070303 ; 081704 ;
摘要
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.
引用
收藏
页码:8739 / 8742
页数:4
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