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Method for preparing dimethylsulfamoyl chloride

A technology for dimethylaminosulfonyl chloride and dimethylaminosulfonyl chloride is applied in the field of preparing dimethylaminosulfonyl chloride, can solve the problems of not conforming to the concept of green chemistry, unsuitable for large-scale production, high production cost, etc., and avoids hydrogen chloride The effect of gas, saving production cost and improving conversion rate

Inactive Publication Date: 2017-09-19
BENGBU CHINA SYNCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method for preparing dimethylaminosulfonyl chloride is to use sulfuryl chloride and dimethylamine hydrochloride as materials, mix and reflux, generate a large amount of hydrogen chloride gas, corrode the production equipment to a certain extent, do not conform to the concept of green chemistry, and have low yield , expensive to produce, not suitable for large-scale production

Method used

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  • Method for preparing dimethylsulfamoyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Throw sulfuryl chloride into a 2L three-necked flask, set up buffer devices front and back, and seal the rear part with water, cool down to 10-20°C in a water bath, feed dimethylamine into the system, the system releases heat, and keep the temperature at 40-50°C. The maximum temperature is below 60°C. Weigh with electronic balance, stop feeding at 440g (ventilation time 4h) and continue stirring, stop reaction after 10min (420g weight increase in the actual weighing reaction bottle), oil bath slowly heats up, reflux overnight at 75°C (during the system heating process, salt Slowly dissolve and clarify, there is a large amount of acid gas, and the system is still clarified, weighing 1000g, distilling at 80°C-90°C under normal pressure to obtain about 200g fractions, and 650g product with a purity of 96% by water pump vacuum distillation. No solid was precipitated during the distillation process, and the final residue was 140 g, calculated as dimethylamine, with a molar y...

Embodiment 2

[0017] Throw sulfuryl chloride into a 2L three-necked flask, set buffer devices front and rear, liquid seal the rear, cool the ice salt to 0-10°C, feed dimethylamine into the system, the system releases heat, and keep the temperature at 40-50°C. The maximum temperature is below 50°C. Weigh with electronic balance, stop feeding at 440g (ventilation time 4h) and continue stirring, stop reaction after 10min (420g weight increase in the actual weighing reaction bottle), oil bath slowly heats up, reflux overnight at 75°C (during the system heating process, salt Slowly dissolve and clarify, there is a large amount of acid gas, and the system is still clarified, weighed 1100g, distilled at 80°C-90°C under normal pressure, and obtained about 150g of fractions, and 800g of product was obtained by water pump vacuum distillation, with a purity of 97.2%. No solid was precipitated during the distillation process, and the final residue of 120 g was calculated as dimethylamine, and the molar...

Embodiment 3

[0019] Throw sulfuryl chloride into a 2L three-necked flask, set up buffer devices front and back, and seal the rear with liquid, cool the ice salt to 0-10°C, feed dimethylamine into the system, the system will release heat, and keep the temperature at 10-20°C. The maximum temperature is below 30°C. Weigh with electronic balance, stop feeding at 440g (ventilation time 4h) and continue stirring, stop reaction after 10min (420g weight increase in the actual weighing reaction bottle), oil bath slowly heats up, reflux overnight at 75°C (during the system heating process, salt Slowly dissolve and clarify, there is a large amount of acid gas, and the system is still clarified, weighed 1384g, and distilled at 80°C-90°C under normal pressure to obtain about 71g of fractions, and 1116g of product was obtained by water pump vacuum distillation with a purity of 98%. No solid was precipitated during the distillation process, and the final residue was 93g, calculated as dimethylamine, and ...

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Abstract

The invention discloses a method for preparing dimethylaminosulfonyl chloride, which relates to the technical field of organic synthesis. Under dry conditions, dimethylamine gas is passed into the sulfonyl chloride liquid, and after the passage is completed, the reaction is refluxed until clarification. Lower the temperature, and distill under normal pressure to obtain the former fraction, and then distill under reduced pressure with a water pump to obtain the product dimethylaminosulfonyl chloride. The average purity of the product dimethylaminosulfonyl chloride of the present invention reaches more than 97%, and the highest molar yield is close to 80%. The yield and purity of the product are guaranteed while shortening the reaction time, so that the synthesis method is suitable for large-scale production.

Description

Technical field: [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing dimethylaminosulfonyl chloride. Background technique: [0002] Dimethylaminosulfonyl chloride is an important raw material for the preparation of Cyazofamid. The field application of Cyazofamid (120116-88-3) has a very high control effect on late blight and downy mildew, and the dosage is 2 times lower than other fungicides. ~38 times, and the medication period is flexible and the duration of effect is long. At present, the method for preparing dimethylaminosulfonyl chloride is to use sulfuryl chloride and dimethylamine hydrochloride as materials, mix and reflux, generate a large amount of hydrogen chloride gas, corrode the production equipment to a certain extent, do not conform to the concept of green chemistry, and have low yield , the production cost is expensive, and it is not suitable for large-scale production. Invention content: [00...

Claims

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Application Information

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IPC IPC(8): C07C381/00
CPCC07C381/00
Inventor 杨青赵士民徐剑霄周威威
Owner BENGBU CHINA SYNCHEM TECH CO LTD
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