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Preparation method of 2-amino-5-sulfydryl-1, 3, 4-thiadiazole

A technology of thiadiazole and mercapto, which is applied in the field of preparation of 2-amino-5-mercapto-1,3,4-thiadiazole, can solve the problems of low yield of the method and high requirements for reaction temperature control, and meet the requirements of The effect of developing demand, shortening the reaction time, and increasing the yield

Pending Publication Date: 2021-10-15
南京硕达生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are relatively few synthetic methods in China, and the common method is high-temperature cyclization of dithiourea. This part has higher requirements for reaction temperature control, and the current method has a low yield, about 80%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation method of 2-amino-5-mercapto-1,3,4-thiadiazole, the operation steps are as follows:

[0022] S1: Prepare the raw material solution: add a certain amount of water to the reaction kettle 1, add hydrochloric acid at a temperature of 10-20°C, stir evenly and add dithiourea in batches to prepare the raw material solution 1 for later use, the quality of dithiourea in water The percentage is 20%, and the molar ratio of dithiourea to hydrochloric acid is 1:2; add a certain amount of water into the reaction kettle 2, then control the temperature at 10-20°C, and add calcium phosphite in batches, the mass percentage of calcium phosphite It is 20%, and it is used as the raw material liquid 2 after mixing evenly; the flow rate of pumps 1 and 2 is calculated according to the molar ratio of calcium phosphite and dithiourea as 0.1:1;

[0023] S2: Set up equipment: use silicon nitride reactor for reaction, plunger pump feeding; the inlet ports of plunger pumps 1 and 2 are ...

Embodiment 2

[0028] A preparation method of 2-amino-5-mercapto-1,3,4-thiadiazole, the operation steps are as follows:

[0029] S1: Prepare the raw material solution: add a certain amount of water to the reaction kettle 1, add hydrochloric acid at a temperature of 10-20°C, stir evenly and add dithiourea in batches to prepare the raw material solution 1 for later use, the quality of dithiourea in water The percentage is 30%, and the molar ratio of dithiourea to hydrochloric acid is 1:3; add a certain amount of water into the reaction kettle 2, then control the temperature at 10-20°C, and add calcium phosphite in batches, the mass percentage of calcium phosphite It is 20%, and it is used as the raw material liquid 2 after mixing evenly; the flow rate of pumps 1 and 2 is calculated according to the molar ratio of calcium phosphite and dithiourea as 0.1:1;

[0030] S2: Set up equipment: use silicon nitride reactor for reaction, plunger pump feeding; the inlet ports of plunger pumps 1 and 2 are ...

Embodiment 3

[0035] A preparation method of 2-amino-5-mercapto-1,3,4-thiadiazole, the operation steps are as follows:

[0036] S1: Prepare the raw material solution: add a certain amount of water to the reaction kettle 1, add hydrochloric acid at a temperature of 10-20°C, stir evenly and add dithiourea in batches to prepare the raw material solution 1 for later use, the quality of dithiourea in water The percentage is 20%, and the molar ratio of dithiourea to hydrochloric acid is 1:3; a certain amount of water is added to the reaction kettle 2, and then the temperature is controlled at 10-20°C, and calcium phosphite is added in batches, the mass percentage of calcium phosphite It is 20% and it is used as raw material solution 2 after mixing evenly; the flow rate of pumps 1 and 2 is calculated according to the molar ratio of calcium phosphite and dithiourea as 0.2:1;

[0037] S2: Set up equipment: use silicon nitride reactor for reaction, plunger pump feeding; the inlet ports of plunger pum...

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Abstract

The invention discloses a preparation method of 2-amino-5-sulfydryl-1, 3, 4-thiadiazole, and particularly relates to a method for producing 2-amino-5-sulfydryl-1, 3, 4-thiadiazole by using a microreactor, the reaction temperature is 80 to 100 DEG C, the reaction time is 0.5 to 1 hour, and the reaction pressure is 100 to 160 psi. The method comprises the following steps: S1, preparing a raw material solution; S2, building equipment: carrying out reaction by using a silicon carbide reactor; S3, carrying out cyclization reaction; and S4, post-treatment: carrying out suction filtration, water washing and drying on the reaction liquid to obtain a product. According to the invention, the traditional preparation method of 2-amino-5-sulfydryl-1, 3, 4-thiadiazole is converted into a Flow mode, and the reaction time is shortened and the reaction yield is improved by strengthening the reaction process and accurately controlling the temperature. Meanwhile, the mode is beneficial to realizing automatic production of products and meeting the industry development requirements.

Description

technical field [0001] The invention relates to the field of pesticide preparation, in particular to a preparation method of 2-amino-5-mercapto-1,3,4-thiadiazole. Background technique [0002] Dithiadiazole compounds have good biological activity. In addition to being widely used in medicine, pesticides, photography, etc., they can also be used as metal complexing agents and corrosion inhibitors. Chemicals are in increasing demand. [0003] At present, there are relatively few synthetic methods in China, and the common method is high-temperature cyclization of dithiourea, which has high requirements for reaction temperature control. The current method has a low yield of about 80%. In order to meet the demands of the modern industry and the demand for continuous production, the present invention adopts the Flow method to strengthen the process and improve the yield while realizing continuous production. Contents of the invention [0004] Based on the technical problems ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D285/135
CPCC07D285/135
Inventor 席亚男张俊
Owner 南京硕达生物科技有限公司
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