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Synthetic method for preparing pure phenyl chloroformate with two-step method

A technology for the synthesis of phenyl chloroformate and its synthesis method, which is applied in the field of synthesis of pure phenyl chloroformate by a two-step method, which can solve the problems of high cost, leakage of phosgene, and environmental pollution, so as to increase yield and prevent leakage , Avoid mass use and the effect of recycling

Inactive Publication Date: 2016-09-21
ANHUI GUANGXIN AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the problems in the prior art that the cost is high, the environment is polluted, and the use of phosgene is easy to cause leakage, etc., and a two-step method is provided to prepare a synthetic method for pure phenyl chloroformate

Method used

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Experimental program
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Effect test

Embodiment 1

[0016] A kind of synthetic method that two-step method prepares pure product phenyl chloroformate mainly comprises the following steps:

[0017] (1) Add 50g of molten phenol and 2.5g of catalyst N,N-dimethylformamide to the reactor, start stirring, and feed 1.06mol of phosgene at 100°C, add activated carbon after the reaction is complete, and add to the reaction Nitrogen was passed into the solution for about 20 minutes, and an automatic ammonia water spraying system was added on the top of the reaction kettle at the same time. If phosgene leaked, the ammonia water spraying system could automatically spray ammonia water to minimize the harm. After the reaction, the crude product phenyl chloroformate was obtained;

[0018] (2) the obtained crude product phenyl chloroformate is obtained through rectification under reduced pressure to obtain pure product phenyl chloroformate.

[0019] The purity of the phenyl chloroformate prepared by the above method is 95.6%, and the yield is 8...

Embodiment 2

[0021] A kind of synthetic method that two-step method prepares pure product phenyl chloroformate mainly comprises the following steps:

[0022] (1) Add 20g of molten phenol and 1g of catalyst N,N-dimethylformamide to the reaction kettle, start stirring, and feed 0.42mol of phosgene at 105°C, add activated carbon after the reaction is complete, and add to the reaction solution Nitrogen was passed into the middle for about 20 minutes, and an automatic ammonia water spraying system was added on the top of the reaction kettle at the same time. If there was a phosgene leakage, the ammonia water spraying system could automatically spray ammonia water to minimize the harm, and the crude product phenyl chloroformate was obtained after the reaction was completed;

[0023] (2) the obtained crude product phenyl chloroformate is obtained through rectification under reduced pressure to obtain pure product phenyl chloroformate.

[0024] The purity of the phenyl chloroformate prepared by th...

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Abstract

The invention provides a synthetic method for preparing pure phenyl chloroformate with a two-step method. The method comprises main steps as follows: (1) phenol in a molten state and a small quantity of a catalyst DMF (dimethyl formamide) are added to a flask, stirring is started, phosgene is introduced at a certain temperature, activated carbon is added after complete reaction, nitrogen is introduced to a reaction solution, and crude phenyl chloroformate is obtained after the reaction ends; (2) obtained crude phenyl chloroformate is subjected to reduced pressure distillation, and pure phenyl chloroformate is obtained. Compared with the prior art, the method has the advantages as follows: aftertreatment is simple, use of large quantities of acid-binding agents and solvents is effectively avoided, no industrial waste water is produced, the cost is relatively low, the method is suitable for industrial production, and meanwhile, possible harm to the phosgene can be reduced through improvement of equipment.

Description

Technical field: [0001] The invention relates to a two-step synthesis method for preparing pure phenyl chloroformate, in particular to the field of pesticide synthesis. Background technique: [0002] Phenyl chloroformate is a corrosive oily liquid, insoluble in water, soluble in ethanol and ether, and easily soluble in petroleum ether. Phenyl chloroformate is an important intermediate in organic synthesis, widely used in chemical synthesis, and can be used as Polymer catalysts, plastic modifiers, fiber treatment agents, and intermediates of pharmaceuticals and pesticides. [0003] The main synthetic method of phenyl chloroformate is the phosgene method at present, and main steps are: (1) phenol is dissolved in chloroform, feeds phosgene under cooling, and the amount of the substance of phosgene is equal to the amount of the substance of phenol (2) Control the reaction temperature at 5-10°C, add the amount of N, N-dimethylaniline dropwise under stirring conditions, and then ...

Claims

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Application Information

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IPC IPC(8): C07C68/02C07C69/96
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杨志伟高焰兵
Owner ANHUI GUANGXIN AGROCHEM
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