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Method for continuously synthesizing O-ethyl-S-sec-butyl thiophosphoryl chloride

A technology of sec-butyl phosphorothioate and di-sec-butyl disulfide is applied in the field of continuous synthesis of O-ethyl-S-sec-butyl phosphorothio chloride, which can solve the problems of low production efficiency, yield and Low purity, cumbersome operation and other problems, to achieve the effect of improving product quality, reducing reaction time, and broad application prospects

Pending Publication Date: 2022-03-22
HEBEI VEYONG BIO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the cumbersome operation of the existing method for preparing ethyl-S-sec-butylphosphoryl thiochloride, low production efficiency and low yield and purity of the prepared ethyl-S-sec-butylphosphoryl thiochloride product problem, the present invention provides a method for continuous synthesis of O-ethyl-S-sec-butylphosphoryl thiochloride

Method used

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  • Method for continuously synthesizing O-ethyl-S-sec-butyl thiophosphoryl chloride
  • Method for continuously synthesizing O-ethyl-S-sec-butyl thiophosphoryl chloride
  • Method for continuously synthesizing O-ethyl-S-sec-butyl thiophosphoryl chloride

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Embodiment 1

[0029] This embodiment provides a method for continuous synthesis of O-ethyl-S-sec-butylphosphoryl thiochloride, comprising the following steps:

[0030] Chlorine gas is continuously fed into the tubular reactor through a mass flow meter at a flow rate of 248.5mL / min, while toluene and di-sec-butyl disulfide are continuously fed through a metering pump at a rate of 6.0g / min and 2.0g / min, respectively. Pass into the tubular reactor, control the reaction time to be 3min, and the reaction temperature is -10°C to obtain the sulfur-based chloride intermediate. Subsequently, the sulfur-based chloride intermediate is connected to the pipe reactor at a position 5 / 9 from the inlet end. The diethyl chlorophosphite that enters is contacted, and the feeding flow rate of diethyl chlorophosphite is 3.5g / min, and the oxidation reaction is continued, and the reaction time is controlled to be 2.5min. The product is collected in a product collection bottle, and the solvent is evaporated , in O-...

Embodiment 2

[0032] This embodiment provides a method for continuous synthesis of O-ethyl-S-sec-butylphosphoryl thiochloride, comprising the following steps:

[0033] Chlorine gas is continuously fed into the tubular reactor through a mass flow meter at a flow rate of 273.4mL / min, while toluene and di-sec-butyl disulfide are continuously fed through a metering pump at a rate of 12.0g / min and 2.0g / min, respectively. Pass into the tubular reactor, control the reaction time to be 2.0min, and the reaction temperature is -5°C to obtain the sulfur-based chloride intermediate. Subsequently, the sulfur-based chloride intermediate is passed through the pipe reactor at a position 1 / 2 from the inlet end. The diethyl chlorophosphite that enters is contacted, and the feeding flow rate of diethyl chlorophosphite is 3.5g / min, continues to carry out oxidation reaction, and control reaction time is 1.8min, and product is collected with product collection bottle, evaporates solvent , in O-ethyl-S-sec-butyl ...

Embodiment 3

[0035] This embodiment provides a method for continuous synthesis of O-ethyl-S-sec-butylphosphoryl thiochloride, comprising the following steps:

[0036] Chlorine gas is continuously fed into the tubular reactor through a mass flow meter at a flow rate of 621.3mL / min, while toluene and di-sec-butyl disulfide are continuously fed through a metering pump at a rate of 40.0g / min and 5.0g / min, respectively. Pass into the tubular reactor, control the reaction time to be 2min, and the reaction temperature is 5°C to obtain the sulfur-based chloride intermediate, and subsequently, the sulfur-based chloride intermediate is passed into the tubular reactor at a position 4 / 7 from the inlet end Diethyl chlorophosphite contacts, and the feeding flow rate of diethyl chlorophosphite is 9.2g / min, continues to carry out oxidation reaction, and the control reaction time is 1.5min, and the product is collected with product collection bottle, evaporates and removes solvent, obtains O-ethyl-S-sec-bu...

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Abstract

The invention relates to the technical field of organic synthesis, and particularly discloses a method for continuously synthesizing O-ethyl-S-sec-butyl thiophosphoryl chloride. The preparation method comprises the following steps: respectively and continuously adding a chlorinating agent, an organic solvent and di-sec-butyl disulfide into a tubular reactor for chlorination reaction to obtain a sulfur chloride intermediate; then, the sulfur chloride intermediate is in contact with chlorinated diethyl phosphite which is continuously introduced, an oxidation reaction continues to be carried out, concentration is carried out, and an O-ethyl-S-sec-butyl thiophosphoryl chloride product is obtained. By adopting continuous reaction, the problem of solvent chlorination is effectively reduced, the content of solvent chloride in the final product is reduced to 0.02% or below, the product quality is effectively improved, recycling of the reaction solvent is facilitated, the hazardous waste treatment cost is reduced, the economic benefit and the environmental benefit are relatively high, the market competitiveness of enterprises is improved, and the method has a wide application prospect. And the method has extremely high popularization and application values.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for continuously synthesizing O-ethyl-S-sec-butylphosphoryl thiochloride. Background technique [0002] Thiazophosphine is a high-efficiency, medium-to-low toxicity, broad-spectrum and safe nematicide developed by Ishihara Corporation of Japan. The agent not only has a broad spectrum of activity against plant parasitic nematodes and pests and their eggs, but also has the activity of killing pests such as aphids, mites, whitefly, thrips and beetles. [0003] O-ethyl-S-sec-butylthiophosphoryl chloride is a key intermediate for the synthesis of thiazophosphine. At present, di-sec-butyl disulfide, phosphorus trichloride and sulfuryl chloride are mainly used as raw materials in industry to synthesize S- sec-butylphosphorothioate dichloride, and then react with ethanol to synthesize O-ethyl-S-sec-butylphosphorothioate chloride, the specific process route is as follo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/20
CPCC07F9/20
Inventor 田学芳赵娜范立攀孙敬东张美丽翟立华孙良侯红欣高永民李志峰贾成国
Owner HEBEI VEYONG BIO CHEM
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