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Method for preparing 1,1,3-trichloroacetone

A technology of trichloroacetone and dichloroacetone, applied in the field of preparing 1,1,3-trichloroacetone, can solve the problems of low yield, long reaction period and the like, and achieve the effect of high yield

Active Publication Date: 2018-11-02
江西天新药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention provides a new method for preparing 1,1,3-trichloroacetone aiming at many technical problems such as long reaction period and low yield in the existing 1,1,3-trichloroacetone synthesis process

Method used

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Examples

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preparation example Construction

[0031] The method for preparing 1,1,3-trichloroacetone provided by the invention has the following specific advantages:

[0032] 1. Compared with the existing catalytic chlorination process using chlorine gas as the chlorination reagent, the present invention uses trichloroisocyanuric acid with lower activity as the reaction raw material, which has high available chlorine content, stable chemical properties, and is easy to transport, store and feed , there is no need to make special design for the operation workshop to use chlorine gas;

[0033] 2. The trichloroisocyanuric acid of the present invention can react rapidly at a relatively high temperature and simultaneously increase the yield of 1,1,3-trichloroacetone.

[0034] The present invention will be described in detail below by way of examples.

[0035] In the following examples, unless otherwise specified, all raw materials used were commercially available.

[0036] The following gas chromatographic analysis conditions...

Embodiment 1

[0042] Add 500 g of dichloroacetone mixture (made by reacting acetone (4.0 mol) and chlorine gas (8.0 mol) at 10° C. for 2 h in a 2500 mL three-necked flask, wherein the GC content of 1,1-dichloroacetone is 70.8% by weight, 1, 3-Dichloroacetone (GC content: 12.3% by weight), 25g of methanesulfonic acid, heating and controlling the internal temperature of the reaction solution to be 115-120°C, adding 100g of trichloroisocyanuric acid to the flask within 10min, and keeping the temperature for 30min after the addition; Then add 50g of trichloroisocyanuric acid to the flask, keep stirring for 30min after adding within 5min; then add 25g of trichloroisocyanuric acid into the flask, keep stirring for 30min after adding within 5min; then add 12.5 g trichloroisocyanuric acid, keep stirring for 30 minutes after adding within 5 minutes, stop the reaction. The 1,1,3-trichloroacetone GC content was 55% by weight. Remove the heat from the reaction, cool down to 45°C naturally, filter with...

Embodiment 2

[0045] Add 500 g of dichloroacetone mixture (made by reacting acetone (4.0 mol) and chlorine gas (7.0 mol) at 5° C. for 2.5 h into a 2500 mL three-necked flask, wherein the GC content of 1,1-dichloroacetone is 67.2% by weight, 1 , 3-dichloroacetone GC content 11.2% by weight), 25g of p-toluenesulfonic acid, heating and controlling the internal temperature of the reaction solution to be 125~130°C, adding 46.8g of trichloroisocyanuric acid to the flask within 30min, after adding Insulate for 10 minutes; then add 46.8g trichloroisocyanuric acid to the flask, keep stirring for 5 minutes after adding within 30 minutes; then add 46.8g trichloroisocyanuric acid to the flask, keep stirring for 5 minutes after adding within 30 minutes; then Add 46.8g of trichloroisocyanuric acid to the flask, and keep stirring for 5 minutes after adding within 30 minutes to stop the reaction. The 1,1,3-trichloroacetone GC content was 54% by weight. Remove the heat from the reaction, cool down naturall...

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Abstract

The invention relates to the field of organic synthesis and discloses a method for preparing 1,1,3-trichloroacetone. The method comprises: in the presence of an acidic catalyst, contacting a raw material containing 1,1-dichloroacetone and / or 1,3-dichloroacetone with symclosene for reaction. The method for preparing 1,1,3-trichloroacetone provided by the invention can achieve the purpose of obtaining 1,1,3-trichloroacetone with high purity and high yield in a short period in a pilot production process or even an industrial production process.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for preparing 1,1,3-trichloroacetone. Background technique [0002] 1,1,3-Trichloroacetone is an important intermediate in the production of folic acid (vitamin B9). Folic acid is a water-soluble vitamin and is the coenzyme of the one-carbon unit transferase system in the biochemical reactions in the human body. It plays a role in the transfer of one-carbon units The role of the body is to promote the growth and reproduction of the body's cells necessary for the substance. [0003] Because the natural folic acid is extremely unstable and easily destroyed by sunlight, temperature, acid-base and other factors, the amount of folic acid that the human body can actually obtain from food is very limited; while the synthetic folic acid can remain stable for a long time and is easily destroyed by the human body. Absorption and high utilization. [0004] 1,1,3-Trichloroacetone ...

Claims

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Application Information

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IPC IPC(8): C07C45/63C07C45/82C07C49/16
CPCC07C45/63C07C45/82C07C49/16
Inventor 余小兵冯正川张先南熊文泉司玉贵
Owner 江西天新药业股份有限公司
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