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A kind of preparation method of deuterated chloroform

A technology of deuterated chloroform and sodium trichloroacetate, which is applied in the field of preparation of deuterated chloroform, can solve the problems of cumbersome process dehydration, poor quality of deuterated chloroform, etc., and achieve obvious economic benefits and reduce the amount of use

Active Publication Date: 2021-04-06
CHENGDU BIOBEL BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

This method is because the calcium trichloroacetate of preparation contains water of crystallization, causes literature to adopt loaded down with trivial details process dehydration, if water is mixed into next step reaction and will make deuterated chloroform mixed with the chloroform that is difficult to separate, the deuterated chloroform that this method prepares is of poor quality , and the yield reported in the literature is only 60%

Method used

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Embodiment 1

[0019] The preparation of embodiment 1 deuterated chloroform

[0020] 370 grams of sodium trichloroacetate and 61.6 grams of calcium oxide, 18.2 grams of heavy water are packed in a 500 milliliter three-necked bottle, a cooling recovery device is installed, and airtight mechanical stirring is heated up to 90 degrees Celsius to react without heavy water in the system, and 209.2 grams of condensed liquid are collected. The yield of crude product is 96.0%. Crude deuterated chloroform was added with 20 g of granular anhydrous calcium chloride, stirred and dried for 0.5 hour, filtered off calcium chloride, and the filtrate was distilled at atmospheric pressure, and the fraction at 60-61° C. was collected to obtain 203.8 g of deuterated chloroform, a colorless transparent liquid. The rate is 97.4%. The combined calculation yield of the two steps is 93.5%.

[0021] Determination of deuteration rate: Accurately weigh 182mg of dimethyl terephthalate into a 100ml volumetric flask, dis...

Embodiment 2

[0022] The preparation of embodiment 2 deuterated chloroform

[0023] 300 grams of sodium trichloroacetate and 49.9 grams of calcium oxide, 14.7 grams of heavy water are packed into a 500 milliliter three-necked bottle, a cooling recovery device is installed, and airtight mechanical stirring is heated up to 95 degrees Celsius to react without heavy water in the system, and 172.0 grams of condensed liquid are collected. The yield of crude product is 97.1%. Add 15 grams of granular deuterated chloroform to the crude product deuterated chloroform and stir and dry for 0.5 hour, filter the calcium chloride, and distill the filtrate at atmospheric pressure, collect the fraction of 60-61 to obtain 166.6 grams of deuterated chloroform as a colorless transparent liquid, the yield 96.9%. The combined calculation yield of the two steps is 94.1%. According to the above method, the deuterium substitution rate is 99.86%.

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Abstract

The invention provides a kind of preparation method of deuterated chloroform, and it comprises the following steps: (1) get sodium trichloroacetate, calcium oxide, heavy water, react at 80~95 ℃, finish reaction to obtain crude product after heavy water reaction is complete; 2) Take the crude product obtained in step (1), dry and separate to obtain deuterated chloroform. The invention uses commonly used cheap chemicals as reagents, has few side reactions, easy separation of reaction products, simple process, high yield and low cost, and has great social and economic benefits.

Description

technical field [0001] The invention belongs to the field of compound synthesis, and in particular relates to a preparation method of deuterated chloroform. Background technique [0002] Deuterated chloroform is a commonly used solvent for NMR detection. With the rapid development of deuterated drugs, deuterated chloroform is also widely used as a deuterated reagent. At present, the preparation method of deuterated chloroform is mainly prepared by reacting trichloroacetophenone, hexachloroacetone or calcium trichloroacetate as raw materials with heavy water under alkali catalysis. The literature (A New Synthesis of Chloroform-d1J.Am.Chem.Soc., 1951,73(2), pp 769–770) reported that trichloroacetic acid and calcium carbonate were used to prepare calcium trichloroacetate, and then the generated trichloroacetic acid was Calcium reacts with heavy water to produce deuterated chloroform. This method is because the calcium trichloroacetate of preparation contains water of crystall...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/363C07C19/04C07B59/00
CPCC07B59/001C07B2200/05C07C17/363C07C19/04
Inventor 广兵谢建董韧涵秦岭彭向阳
Owner CHENGDU BIOBEL BIOTECHNOLOGY CO LTD
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