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Preparation method of 1, 1, 3-trichloroacetone

A technology of trichloroacetone and chlorine gas, which is applied in the field of organic synthesis intermediate preparation, can solve the problems such as cumbersome processing of intermediate products, unfavorable industrialized production, etc., and achieves the effects of improving purity and increasing reaction temperature.

Active Publication Date: 2018-07-27
戚一文
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method can obtain products with higher purity, but the treatment of intermediate products is relatively cumbersome, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 5.8g (0.1mol) of acetone and 30mL of chlorobenzene into the reaction flask, add 0.5g of bipyridine, start stirring, control the temperature at 20-30°C, then pass in about 14.2g of chlorine gas to react, and react for 2 hours. Then add 0.5 g of tetracyano-p-benzoquinone dimethane, control the temperature at 50-60° C., continue to introduce about 7.1 g of chlorine gas, and continue to react for 5 hours. Then the solvent was distilled off under reduced pressure to obtain a solid residue. Add 40mL of dichloromethane and 20mL of petroleum ether to the residue, raise the temperature to reflux, keep it warm for 1 hour, slowly cool down to 5-10°C, filter with suction, and filter the cake with a small amount of petroleum After washing with ether, the filter cake was collected and dried to obtain 13.4 g of a solid product with a GC purity of 97.8% and a yield of 83.2%.

Embodiment 2

[0023] Put 5.8g (0.1mol) of acetone and 30mL of chlorobenzene into the reaction flask, add 0.5g of bipyridine, start stirring, control the temperature at 20-30°C, then pass in about 14.2g of chlorine gas to react, and react for 2 hours. Then add 0.5g of 1,1-diphenyl-2-trinitrophenylhydrazine, control the temperature at 50-60°C, continue to pass in about 7.1g of chlorine gas, and continue to react for 5 hours. Then the solvent was distilled off under reduced pressure to obtain a solid residue. Add 40mL of dichloromethane and 20mL of petroleum ether to the residue, raise the temperature to reflux, keep it warm for 1 hour, slowly cool down to 5-10°C, filter with suction, and filter the cake with a small amount of petroleum After washing with ether, the filter cake was collected and dried to obtain 12.8 g of a solid product with a GC purity of 96.8% and a yield of 79.4%.

Embodiment 3

[0025] Put 5.8g (0.1mol) of acetone and 30mL of chlorobenzene into the reaction flask, add triethylamine, start stirring, control the temperature at 20-30°C, and then pass in about 14.2g of chlorine gas to react. After 45 minutes of reaction, Add 0.5g of 1,1-diphenyl-2-trinitrophenylhydrazine, control the temperature at 50-60°C, continue to pass in about 7.1g of chlorine gas, and continue to react for 5 hours. Then the solvent was distilled off under reduced pressure to obtain a solid residue. Add 40mL of dichloromethane and 20mL of petroleum ether to the residue, raise the temperature to reflux, keep it warm for 1 hour, slowly cool down to 5-10°C, filter with suction, and filter the cake with a small amount of petroleum After washing with ether, the filter cake was collected and dried to obtain 11.1 g of a solid product with a GC purity of 94.8% and a yield of 68.9%.

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PUM

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Abstract

The invention discloses a preparation method of 1, 1, 3-trichloroacetone. The preparation method comprises (1) under the existence of additives, subjecting acetone and chlorine for chlorination to obtain chlorinated intermediate solution; (2) adding radical scavenger into the obtained chlorinated intermediate solution, continuing to inletting chlorine for reaction under heating conditions, and processing reaction products to obtain the 1, 1, 3-trichloroacetone. The preparation method of the 1, 1, 3-trichloroacetone is implemented through two steps, and during the second step, a certain amountof the radical scavenger is added, so that selectivity and purity of the 1, 1, 3-trichloroacetone can be improved.

Description

technical field [0001] The invention belongs to the field of preparation of organic synthesis intermediates, and in particular relates to a preparation method of 1,1,3-trichloroacetone. Background technique [0002] 1,1,3-Trichloroacetone is a colorless, transparent liquid with a strong pungent odor. It is an important chemical intermediate and can be used in organic synthesis, preparation of medicines, pesticides, spices and dyes, etc. The most important application is for the synthesis of folic acid. [0003] At present, the main methods for preparing 1,1,3-trichloroacetone are direct chlorination of acetone and stepwise chlorination. The Chinese patent with the publication number CN1047853A proposes a method for preparing 1,1,3-trichloroacetone by catalyzing the chlorine chlorination of acetone with triethylamine and diethylamine. The reaction time of this method is 10-20 hours, and the reaction cycle is longer , the content of 1,1,3-trichloroacetone in the product is o...

Claims

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Application Information

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IPC IPC(8): C07C49/16C07C45/63
CPCC07C45/63C07C49/16
Inventor 石磊任炼军孙嫚嫚
Owner 戚一文
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