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Method for preparing 1-chloro-1-acetylcyclopropylamine by continuous flow reaction

A kind of cyclopropylamine and reaction technology, which is applied in the field of pesticide intermediate preparation to achieve the effects of reducing contact time and improving yield

Inactive Publication Date: 2019-03-08
DALIAN QIKAI MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction must use a strong alkali sodium hydroxide aqueous solution, and a certain reaction temperature is required.

Method used

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  • Method for preparing 1-chloro-1-acetylcyclopropylamine by continuous flow reaction
  • Method for preparing 1-chloro-1-acetylcyclopropylamine by continuous flow reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Mix 3,5-dichloro-2-pentanone and chloroform to form a solution with a mass concentration of 25%, preheat to 30-40°C, and mix tetramethylammonium chloride, NaOH, H2O with a mass ratio of 4.3:20 : 80 into an aqueous solution. Two metering pumps are used to pump the organic matter and the aqueous solution respectively, and the speeds are 4.4g / min and 4.3g / min respectively. The reaction residence time is 10 seconds, the reaction temperature is 55-58° C., and the reaction liquid is rapidly cooled to 20-30° C. through a condenser for oil-water separation. The oil layer was analyzed by GC; the conversion of the raw materials was complete, the purity of the product after deducting the solvent was 98.8%, and the fractional product content of the external standard was 19.7%. Quantitative yield 97.5%. The reaction material was collected for 24 hours, the oil layer was separated, washed with water, and the solvent was distilled off to obtain 1183 g of a colorless oil layer with a...

Embodiment 2

[0025] Mix 3,5-dichloro-2-pentanone and chloroform to form a solution with a mass concentration of 25%, preheat to 30-40°C, and mix tetramethylammonium chloride, NaOH, H2O with a mass ratio of 4.3:20 : 80 into an aqueous solution. Two metering pumps are used to pump the organic matter and the aqueous solution respectively, and the speeds are 4.4g / min and 4.3g / min respectively. The reaction residence time is 10 seconds, the reaction temperature is 40-45° C., and the reaction liquid is quickly cooled to 20-30° C. through the condenser for oil-water separation. The oil layer was analyzed by GC; the remaining 6% was deducted from the solvent raw material, the product purity was 93.8%, and the product content of the external standard was 18.2%. Quantitative yield 90%.

Embodiment 3

[0027] Mix 3,5-dichloro-2-pentanone and chloroform to form a solution with a mass concentration of 25%, preheat to 30-40°C, and mix tetramethylammonium chloride, NaOH, H2O with a mass ratio of 4.3:30 : 70% water to make a solution. Two metering pumps are used to pump the organic matter and the aqueous solution respectively, and the speeds are 4.4g / min and 1.9g / min respectively. The reaction residence time is 10 seconds, the reaction temperature is 55-58° C., and the reaction liquid is rapidly cooled to 20-30° C. through a condenser for oil-water separation. GC analysis; after deducting the remaining 10% of the solvent raw material, the product purity is 89.1%, and the external standard fractional product content is 17.2%. The quantitative yield was 85%.

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Abstract

The invention discloses a method for preparing 1-chloro-1-acetylcyclopropylamine by continuous flow reaction, and belongs to the technical field of fine chemical engineering preparation processes. Themethod comprises the following steps: simultaneously pumping a 3,5-dichloro-2-pentanone and chloroform mixed solution, a sodium hydroxide aqueous solution and a tetrabutylammonium chloride mixed solution in a continuous flow device by a metering pump, and after completing reaction at the temperature of 50-60 DEG C, transferring the mixed solution to a low-temperature region and quenching the mixed solution. A continuous flow reactor replaces kettle type reaction, the time of contact between a product and alkali is shortened, side products such as tar are reduced, and the yield is increased.

Description

technical field [0001] The invention relates to a method for preparing a pesticide intermediate, in particular to a method for preparing 1-chloro-1-acetylcyclopropylamine in a continuous flow mode, and belongs to the technical field of fine chemical preparation technology. Background technique [0002] 1-Chloro-1-acetylcyclopropylamine is mainly used to synthesize prothioconazole, and it is also an intermediate in the synthesis of other pesticides. Prothioconazole is a broad-spectrum fungicide, mainly used for disease control of wheat, barley, rice, rape and other crops. The compound can be quickly absorbed in the animal body and excreted out of the body, has no accumulation, and has low toxicity to humans and animals. It can be rapidly degraded in plants and soil, and has no pollution to the environment. [0003] The existing technology is mainly limited by the low yield, such as Chinese patent: 201410520401X small test yield is 80%, and the yield is reduced by 10-15% whe...

Claims

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Application Information

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IPC IPC(8): C07C45/61C07C49/327
CPCC07C45/61C07C2601/02C07C49/327
Inventor 苑峰张洪学杨永正孙立芹
Owner DALIAN QIKAI MEDICAL TECH
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