Preparation method of prothiocarb

A technology of procarbocarb and benzyl halide, which is applied in the field of pesticide preparation, can solve the problems of high content of impurity dibenzyl disulfide, cumbersome operation process of procarbocarb, large amount of wastewater, etc., and achieve easy and stable process operation The effect of control, short preparation reaction time and low processing cost

Pending Publication Date: 2022-07-01
CAC NANTONG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a preparation method of procarbocarb, the method of the present invention can effectively solve the complicated operation process, long reaction time, excessive waste water and the problem of obtaining procarbocarb in the prior art. The problem of high content of impurity dibenzyl disulfide in benzalt

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  • Preparation method of prothiocarb
  • Preparation method of prothiocarb
  • Preparation method of prothiocarb

Examples

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Embodiment 1

[0042] In the present embodiment, by the following method to prepare procyridone, specifically comprises the following steps:

[0043] Set up a four-necked flask reaction device equipped with a gas guide, a bubbler, a stirring paddle and a thermometer and a tail gas absorption device for sodium hydroxide solution, weigh 99.76g (0.976mol) (content 99%) of di-n-propylamine, and cool it to 10 ℃, introduced 26.97g (0.440mol) (content 98%) carbon oxysulfide, the ventilation time was 1h, the whole process temperature was 10-20℃, after the ventilation was over, the system was heated to 25℃, and 54.98g (0.430mol) was added dropwise. (content 99%) benzyl chloride, dripping time 1h, whole process temperature 25-30 ℃, after the end of dripping, sample analysis after 25-30 ℃ incubating for 3h, HPLC analysis of benzyl chloride content is 0.5119%, benzyl chloride The content was 93.0803%, and the reaction was completed.

[0044] After adding 41.6g of water to the system, the temperature wa...

Embodiment 2

[0046] In the present embodiment, by the following method to prepare procyridone, specifically comprises the following steps:

[0047] Set up a four-necked flask reaction device equipped with a gas guide, a bubbler, a stirring paddle and a thermometer and a tail gas absorption device for sodium hydroxide solution, weigh 101.09g (0.989mol) (content 99%) of di-n-propylamine, and cool it to 13 ℃, feed 27.71g (0.452mol) (content 98%) carbon oxysulfide, the ventilation time is 50min, the whole process temperature is 10-20 ℃, after the ventilation is over, the system is heated up to 25 ℃, and 54.98g (0.430mol) is added dropwise (content 99%) benzyl chloride, dripping time 1h, whole process temperature 25-30 ℃, after the end of dripping, incubate at 25-30 ℃ for 3h, sample and analyze, the content of benzyl chloride by HPLC analysis is 0.4263%, and the benzyl chloride is 0.4263%. The content was 93.8094%, and the reaction was completed.

[0048] After adding 41.6g of water to the sys...

Embodiment 3

[0050] Set up a four-necked flask reaction device equipped with a gas guide, a bubbler, a stirring paddle and a thermometer, and a tail gas absorption device for sodium hydroxide solution, weigh 103.23g (1.01mol) (content 99%) of di-n-propylamine, and cool it to 13 ℃, introduced 28.81g (0.47mol) (content 98%) carbon oxysulfide, the ventilation time was 1h, the whole process temperature was 10-20℃, after the ventilation was over, the system was heated to 25℃, and 54.98g (0.430mol) was added dropwise. (content 99%) benzyl chloride, dripping time 1h, whole process temperature 25-30 ℃, after the end of dripping, sample analysis after 25-30 ℃ incubating for 3h, HPLC analysis of benzyl chloride content is 0.4039%, benzalkonium chloride The content was 93.8831%, and the reaction was completed.

[0051] After adding 41.6g of water to the system, the temperature was raised to 45°C, acidified to pH=1.55 with 32% hydrochloric acid solution, the whole process temperature was 45-50°C, the ...

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Abstract

The invention provides a preparation method of prothiocarb, which comprises the following steps: introducing carbon oxysulfide into a di-n-propylamine solution, adding benzyl halide after the introduction is finished, carrying out heat preservation reaction after the addition is finished, adding water into the system after the reaction is finished, heating, acidifying, stirring, standing, separating liquid, washing an organic phase with water twice, and distilling to obtain the product prothiocarb with the purity of more than 98%, the yield is greater than 92%, and the content of impurity dibenzyl disulfide is lower than 0.04%. According to the preparation method disclosed by the invention, water or other organic solvents are not used during preparation reaction, the operation is simple, safe and controllable, the reaction time is short, the preparation yield is high, the product purity is high, and the content of impurity dibenzyl disulfide in the product is low; and the unreacted raw material di-n-propylamine can be recycled, so that less organic waste liquid is generated, and the three-waste treatment capacity and cost are reduced.

Description

technical field [0001] The invention belongs to the technical field of pesticide preparation, and in particular relates to a preparation method of benflux. Background technique [0002] Prosulfocarb, namely S-benzyldipropylthiocarbamate, is a thiocarbamate selective systemic soil treatment herbicide. Benzopyr is a carbamate herbicide, its mechanism of action is a lipid synthesis inhibitor, it can be used for weeding in rice transplanting fields and direct seeding fields, and can effectively control grass weeds, sedge weeds and broad-leaved weeds Grasses, such as barnyardgrass, sagebrush, horsetan, foxtail, paspalum, oxtenoid, etc; Weeds such as Lilac Polygonum, Cigu genus, Field grass genus, Yujiuhua family genus, Rush genus and Jiejie grass, etc., have special effects on Duckweed. [0003] The reported methods for the preparation of procarbodan are mainly divided into two ways. One is to prepare procyopalan through amines and sulfur-containing intermediates. For example ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/04
CPCC07C333/04
Inventor 薛武平陈亮王海水石阳阳佘颖颖
Owner CAC NANTONG CHEM
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