Method for Small-Scale Production of Deuterochloroform.
Method for Small-Scale Production of Deuterochloroform.
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小规模生产氘代氯仿的方法。
DOI：
10.1021/acs.joc.8b01018
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发表时间：
2018
期刊：
影响因子：
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通讯作者：
Schomaker,JenniferM
中科院分区：
文献类型：
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作者：
Tansukawat,NathaD;See,AlyaaE;Jiranuntarat,Sadudee;Corbin,JoshuaR;Schomaker,JenniferM
氘代氯仿（CDCl 3）是核磁共振（NMR）分析中常用的氘代溶剂。以安全和廉价的方式合成大量的CDCl 3用于研究用途和大型本科生有机实验室是有吸引力的。在此，我们描述了一种方便的实验室规模的制备CDCl 3，采用还原和脱羧六氯-2-丙酮（HCP）催化的各种吡啶。PVP催化剂通过多轮循环提供更清洁的反应和更高的催化剂稳定性，证明其与吡啶相比成本更高。
Deuterochloroform (CDCl3) is a common deuterated solvent for nuclear magnetic resonance (NMR) analyses. The synthesis of significant amounts of CDCl3for 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 CDCl3that 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.