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Thioformamide, and preparation method and application thereof

A thioformamide and formamide technology, applied in the direction of organic chemistry and the like, can solve the problems of high consumption of raw materials, high price of tetrahydrofuran, low yield, etc., and the pressure and temperature conditions are easy to achieve, the preparation process is safe and controllable, and the preparation simple method effect

Inactive Publication Date: 2020-02-25
JIANGSU NOON CROP SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis process of thioformamide is to react with formamide and phosphorus pentasulfide as raw materials. During the reaction, impurities such as phosphorus pentoxide are easily formed to adhere to the wall, forming impurities, which is not conducive to the reaction; moreover, the reaction system often uses tetrahydrofuran (THF) is used as a solvent. On the one hand, tetrahydrofuran is expensive and the cost is high; on the other hand, it is necessary to ensure a completely anhydrous environment. The drying process of THF is complicated and difficult
In short, the synthesis process has low yield, high production cost, large consumption of raw materials, and produces a large amount of phosphorus-containing wastewater and toxic hydrogen sulfide gas. The production process is unsafe, unfavorable to the environment, and the environmental protection disposal cost is extremely high.

Method used

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  • Thioformamide, and preparation method and application thereof

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preparation example Construction

[0018] The first aspect of the present invention provides the preparation method of thioformamide, it may further comprise the steps:

[0019] Using carbon disulfide and formamide as raw materials, under the catalysis of an organic base, react for 6-8 hours under the conditions of a pressure of 3-5 MPa and a temperature of 140-160°C to generate thioformamide, as shown in the following formula (1) Show.

[0020]

[0021] Preferably, the reaction process is carried out in an autoclave. The reaction pressure of the present invention is 3-5 MPa, and the reaction can be carried out under low pressure conditions without expensive high-pressure equipment. The requirements for equipment are relatively low, and the reaction process is safe and controllable.

[0022] The post-processing of the present invention is simple, and the product is easy to separate. Specifically, after the reaction is completed, the autoclave is cooled to below 20° C., and the generated carbon dioxide gas is...

Embodiment 1

[0029] In a 2000ml autoclave (design pressure is 10MPa) equipped with agitator, inner coil condenser, pressure gauge and thermometer, add a certain amount of sodium methoxide, cover the lid of the kettle and do a safety inspection according to regulations. After replacing with nitrogen, add 760g of carbon disulfide and 90g of formamide, after the addition of the raw materials, fill the tank with nitrogen to raise the pressure to 3MPa, and close the nitrogen inlet valve. The temperature was raised to 140°C at a uniform rate within 1 hour for reaction, and the pressure of the kettle was kept at 3-5 MPa. Insulate and react at a temperature of 140-160° C. for 6-8 hours to generate thioformamide. Stop heating, pass cooling water through the inner coil to cool down to below 20°C, open the exhaust pipe to release the pressure to normal pressure, discharge the generated carbon dioxide gas, close the exhaust pipe, and pressurize the reaction liquid with nitrogen gas from the discharge ...

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Abstract

The invention discloses a thioformamide, and a preparation method and an application thereof. Carbon disulfide and formamide which are used as raw materials are reacted under a pressure of 3-5 MPa under the catalytic action of an organic alkali to generate thioformamide, and the thioformamide is rectified and collected after the reaction is finished. The thioformamide prepared in the invention canbe used as an thiabendazole intermediate to synthesize thiabendazole which is applied to the fields of sterilization, corrosion prevention, fresh keeping and the like. The preparation method has theadvantages of simplicity, mild reaction conditions, safety, controllability, low production cost, high yield, no generation of wastewater or toxic gases, and reduction of environmental pollution.

Description

technical field [0001] The invention relates to the field of chemical material synthesis, in particular to thioformamide, a preparation method of thioformamide and the application of thioformamide as a thiabendazole intermediate. Background technique [0002] Thioformamide is the key intermediate of thiabendazole and also an important fine chemical product. [0003] At present, the synthesis process of thioformamide is to react with formamide and phosphorus pentasulfide as raw materials. During the reaction, impurities such as phosphorus pentoxide are easily formed to adhere to the wall, forming impurities, which is not conducive to the reaction; moreover, the reaction system often uses tetrahydrofuran (THF) as a solvent, tetrahydrofuran is expensive on the one hand, and the cost is higher; on the other hand, it is necessary to ensure a completely anhydrous environment, and the THF drying process is more complicated and difficult. In short, the synthesis process has low yie...

Claims

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Application Information

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IPC IPC(8): C07C327/42C07D417/04
CPCC07C327/42C07D417/04
Inventor 孟宪锋
Owner JIANGSU NOON CROP SCI CO LTD
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