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Synthetic method of phenyl chloroformate as pesticide intermediate

A technology for the synthesis of phenyl chloroformate, which is applied to the preparation of phosgene or haloformate, organic chemistry, etc., can solve the problems of high production cost, complicated post-treatment, and large amount of waste water, and achieve low cost and high post-treatment Simple, easy-to-control reaction effects

Inactive Publication Date: 2016-11-09
ANHUI GUANGXIN AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The post-treatment of this method is complicated, a large amount of solvent needs to be recovered, the amount of waste water generated is large, and a large amount of N,N-dimethylaniline is used as an acid-binding agent, and the production cost is high.
[0004] There is currently disclosed a solvent-free method for the synthesis of phenyl chloroformate used as a pesticide intermediate. Directly add molten phenol to a small amount of catalyst, pass through light at high temperature, and then obtain benzene chloroformate with a content greater than 98% by rectification under r

Method used

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  • Synthetic method of phenyl chloroformate as pesticide intermediate

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Comparison scheme
Effect test

Embodiment 1

[0023] First, add 200L tetrahydrofuran into the reaction kettle, dissolve 94Kg phenol in it and keep stirring;

[0024] Next, add 40Kg sodium hydroxide in the reactor after above-mentioned stirring, constantly stir reactor, the time is 1h, and one side of stirred reactor connects circulating refrigerator, and the outside of described stirred reactor is provided with jacket, and described stirred reactor The outer wall is provided with a temperature control pipeline, the temperature control pipeline is connected with a circulating freezer, the temperature control pipeline is located in the jacket of the stirred reactor, and a thermometer is inserted at the top of the stirred reactor;

[0025] First turn on the circulating freezer again, lower the temperature of the stirred reactor to 0°C, then add triphosgene to the stirred reactor, and the amount of triphosgene added is 297Kg, and simultaneously add the catalyst to the stirred reactor, and the reaction time is After 12 hours, ...

Embodiment 2

[0031] First, add 200L tetrahydrofuran into the reaction kettle, dissolve 94Kg phenol in it and keep stirring;

[0032] Next, add 40Kg sodium hydroxide in the reactor after above-mentioned stirring, constantly stir reactor, the time is 1h, and one side of stirred reactor connects circulating refrigerator, and the outside of described stirred reactor is provided with jacket, and described stirred reactor The outer wall is provided with a temperature control pipeline, the temperature control pipeline is connected with a circulating freezer, the temperature control pipeline is located in the jacket of the stirred reactor, and a thermometer is inserted at the top of the stirred reactor;

[0033] First turn on the circulating freezer again, lower the temperature of the stirred reactor to 0°C, then add triphosgene to the stirred reactor, and the amount of triphosgene added is 298Kg, and simultaneously add the catalyst to the stirred reactor, and the reaction time is After 12 hours, ...

Embodiment 3

[0039] First, add 200L tetrahydrofuran into the reaction kettle, dissolve 94Kg phenol in it and keep stirring;

[0040] Next, add 40Kg sodium hydroxide in the reactor after above-mentioned stirring, constantly stir reactor, the time is 1h, and one side of stirred reactor connects circulating refrigerator, and the outside of described stirred reactor is provided with jacket, and described stirred reactor The outer wall is provided with a temperature control pipeline, the temperature control pipeline is connected with a circulating freezer, the temperature control pipeline is located in the jacket of the stirred reactor, and a thermometer is inserted at the top of the stirred reactor;

[0041] First turn on the circulating freezer again, lower the temperature of the stirred reactor to 0°C, then add triphosgene to the stirred reactor, and the amount of triphosgene added is 298Kg, and simultaneously add the catalyst to the stirred reactor, and the reaction time is After 12 hours, ...

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Abstract

The invention provides a synthetic method of phenyl chloroformate as a pesticide intermediate. The method comprises the following steps: adding tetrahydrofuran in a reaction vessel, dissolving phenol and continuously stirring the materials; adding sodium hydroxide in the stirred reaction vessel, continuously stirring the materials in the reaction vessel; reducing the temperature of the reaction vessel, then adding triphosgene in the reaction vessel, taking a center control sample; finally employing nitrogen to expel gas, and performing underpressure distillation to obtain phenyl chloroformate. The method has the advantages of simple post-treatment, low cost, and easy control of reaction generation.

Description

technical field [0001] The invention relates to the production field of fine chemicals, in particular to a method for synthesizing phenyl chloroformate used as a pesticide intermediate. Background technique [0002] Phenyl chloroformate is an important fine chemical intermediate, which is widely used in chemical synthesis and can be used as a polymerization catalyst, plastic modifier, fiber treatment agent, and intermediate of medicine and pesticide. [0003] The main synthesis method of phenyl chloroformate is the phosgene method. Dissolve phenol in chloroform, pass through phosgene under cooling, make the ratio of the absorbed phosgene amount to phenol and other substances, and add other substances dropwise under stirring at 5-10°C The amount of N,N-dimethylaniline. Then dilute with cold water, separate the oil layer, and wash with dilute hydrochloric acid and water successively. After drying with anhydrous calcium chloride, distill to recover chloroform, and then rectif...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/02
CPCC07C68/02C07C69/96
Inventor 黄金祥过学军吴建平胡明宏杨亚明程伟家李红卫徐小兵高焰兵戴玉婷
Owner ANHUI GUANGXIN AGROCHEM
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