Method for preparing deuterochloroform

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

Active Publication Date: 2018-12-28
CHENGDU BIOBEL BIOTECHNOLOGY CO LTD
View PDF3 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

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%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a method for preparing deuterochloroform. The method comprises the following steps: (1) enabling sodium trichloroacetate, calcium oxide and heavy water to react at 80-95 DEG C,and terminating the reaction after the heavy water completely react so as to obtain a crude product; (2) drying and separating the crude product obtained in the step (1), thereby obtaining deuterochloroform. As reagents are cheap chemicals which are common and easy to use, the method is small in side reaction, easy in reaction product separation, simple in process, high in yield, low in cost and great in social and economic benefit.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap