A kind of preparation method of deuterated chloroform

A technology of deuterated chloroform and equation, applied in the field of preparation of deuterated chloroform, can solve the problems of inconvenient transportation and high price, and achieve the effects of easy separation and purification, low cost and few impurities

Active Publication Date: 2019-11-05
宁波萃英化学技术有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are disadvantages such as high price and inconvenient transportation

Method used

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  • A kind of preparation method of deuterated chloroform
  • A kind of preparation method of deuterated chloroform

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Experimental program
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Effect test

Embodiment 1

[0016] Preparation of deuterated chloroform

[0017] Add 200 grams of hexachloroacetone and 30 grams of calcium oxide into a 500 ml three-necked flask with a reflux condenser, add 10 grams of heavy water dropwise while stirring, and complete the dropwise addition in about 10 minutes. Raise the temperature to 110°C for about 8 hours, and the reaction is over. , The reaction was changed to a distillation device, and the fraction at 60-61° C. was collected to obtain 115 grams of colorless transparent liquid with a yield of 95.8%.

[0018] Deuteration rate of deuterated chloroform

[0019] Accurately weigh 182mg of dimethyl terephthalate DMT and add it to a 100ml volumetric flask, dissolve it in 100ml of anhydrous methanol, after it is completely dissolved, take 1ml of the solution in the LC-MS sample bottle, and volatilize completely in an oven at 40°C. Then add 600ul deuterated chloroform to dissolve completely 1 H-NMR. The measured deuterium substitution rate is 99.85%.

Embodiment 2

[0021] Preparation of deuterated chloroform

[0022] Add 220 grams of hexachloroacetone and 28 grams of calcium oxide into a 500 ml three-neck flask with a reflux condenser, add 10 grams of heavy water dropwise while stirring, and the addition is completed in about 10 minutes, and the temperature is raised to 100 degrees for about 8 hours, and the reaction is over. , The reaction was changed to a distillation device, and the 60-61 ° C fraction was collected to obtain 110 grams of deuterated chloroform, with a yield of 91.7%.

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Abstract

The invention discloses a preparation method of deuterochloroform. The preparation method comprises the following steps: with hexachloroacetone, calcium oxide and heavy water as raw materials, reacting at a temperature of 80-120 DEG C; after the reaction, collecting fraction under normal pressure and at 60-61 DEG C to obtain deuterochloroform. The method has the advantages of simple technology, high yield and low cost, and can effectively break the status quo of depending on imported deuterochloroform.

Description

technical field [0001] The invention relates to a preparation method of deuterated chloroform, in particular to a preparation method of deuterated chloroform. Background technique [0002] Deuterated chloroform is the most commonly used solvent for NMR detection. Its main method is to prepare by reacting trichloroacetophenone with heavy water under the catalysis of deuterohaloform Synthesis.la A New Preparation of Chloroform-d, Investigation Of The Deuterohaloform Synthesis, 1951,73; 770-771 ), the method yield is higher, but the atom utilization rate is low, and the raw material trichloroacetophenone is expensive and causes higher cost. In recent years, Liu Hongyu has invented a method (CN103408413B) for preparing deuterated chloroform by reacting hexachloroacetone in heavy water under the catalysis of potassium carbonate, but it is found through experiments that the method has many impurities and low yield. At present, domestic deuterated chloroform mainly relies on impo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/361C07C19/04
CPCC07B2200/05C07C17/361C07C19/04
Inventor 吴涛高章华宋小华毛鸿岗
Owner 宁波萃英化学技术有限公司
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