The synthetic method of cartap

A synthetic method, the technology of cartap, is applied in a new synthetic field, which can solve the problems of safety production and environmental protection risks, low utilization rate of raw material atoms, low yield, etc., and achieve high processing cost, high environmental capacity requirements, and high operational efficiency. easy effect

Active Publication Date: 2018-06-19
仪征市海帆化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The above-mentioned processes all have disadvantages such as lengthy route, complicated operation, low yield, and low utilization rate of raw material atoms.
In particular, the use of highly toxic sodium cyanide in the cyanidation reaction brings great risks to safe production and environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0034] In a 1000ml four-neck flask equipped with a mechanical stirrer, an ice-salt ethanol bath, an exhaust gas absorption device and a thermometer, add 300g of a 20% sodium hydroxide aqueous solution (1.50mol) under stirring, and when the temperature drops to 0°C , Add dropwise 50g of ammonia solution (0.88mol) with a mass fraction of 30% in the system, and control the rate of addition so that the temperature of the system does not exceed 15°C. After the dropwise addition was completed, 50 g (0.83 mol) of carbon oxysulfide gas was slowly introduced. Control the ventilation rate and control the system temperature not to exceed 30°C. After aeration, remove the ice-salt ethanol bath and stir at room temperature for 30 minutes.

[0035] Add 60 g (0.38 mol) of chloride into the system, raise the temperature of the water bath to 60° C., and keep the reaction for 15 hours. After the heat preservation reaction is finished, cool down with an ice-salt ethanol bath, add 200g (1.97mol)...

example 2

[0038] In a 1000ml four-necked flask equipped with a mechanical stirrer, an ice-salt ethanol bath, an exhaust gas absorption device and a thermometer, add 500g of methanol under stirring, and when the temperature drops to 0°C, feed 70g (4.12mol) of liquid ammonia into the system . Immediately, 50 g (0.83 mol) of carbon oxysulfide gas was slowly introduced. Control the ventilation rate and control the system temperature not to exceed 30°C. After aeration, remove the ice-salt ethanol bath and stir at room temperature for 30 minutes.

[0039] Add 60 g (0.38 mol) of chloride into the system, and stir at room temperature for 24 hours. After the end, cool down with an ice salt ethanol bath, dropwise add 350g (3.45mol) of concentrated hydrochloric acid with a mass fraction of 36% within the temperature range of 0-10°C in the system, after the dropwise addition, continue to drop to minus 0°C with ice salt ethanol , and kept stirring for 1 hour.

[0040] Filter with a Buchner funne...

example 3

[0042]In a 1000ml four-necked flask equipped with a mechanical stirrer, ice-salt ethanol bath, tail gas absorption device and thermometer, add 300g of sodium ethylate ethanol solution (1.32mol) with a mass fraction of 30% under stirring, and when the temperature drops to 10°C 15 g of 40% liquid ammonia ethanol solution (0.35 mol) was added dropwise to the system, and the rate of addition was controlled so that the temperature of the system did not exceed 15°C. After the dropwise addition was completed, 20 g (0.33 mol) of carbon oxysulfide gas was slowly introduced. Control the ventilation rate and control the system temperature not to exceed 10°C. After aeration, the ice-salt ethanol bath was removed, and the system was stirred at room temperature for 30 minutes, and the system became a cloudy solution.

[0043] Add 23g (0.15mol) chloride and 0.5g tetrabutylammonium bromide into the system, stir at room temperature for 1 hour, then raise the temperature of the water bath to r...

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Abstract

The invention provides a synthesis method of cartap, and relates to a synthesis method of 1,3-bis(carbamyl sulfonium)-2-(N,N-dimethylamino) propane hydrochloride. An original medicine of cartap is prepared from carbon oxysulfide, ammonia and 1-(N,N-dimethylamino)-2,3-propylene dichloride (chloride for short) through a one-pot method in an alkaline solution. By the adoption of the one-pot method for reaction step by step to prepare the cartap, the synthesis method has the advantages of low equipment investment, low energy consumption, easiness and convenience for operation and substantial improvement of the conversion rate. According to the synthesis method, the use of organic raw materials such as sodium thiosulfate (sodium thiosulfate) and sodium cyanide is avoided, so that generation of a large amount of sewage containing sodium sulfite and sodium cyanide is avoided. The synthesis method substantially increases the selectivity and the conversion rate in a reaction process, thus improving the production efficiency and greatly reducing the production cost.

Description

technical field [0001] The invention proposes a brand-new synthesis method of the insecticide cartap. Background technique [0002] Cartap, also known as Badan, Paidan, foreign trade name Cartap. It is an insecticide developed by Japan's Takeda Pharmaceutical Co., Ltd. based on the animal toxin-nereistoxin. It is a new broad-spectrum insecticide with high efficiency, low toxicity and broad spectrum for controlling pests such as rice stem borers, tea leaves, fruit trees and vegetables. Low toxicity to humans and animals, safe and convenient to use. [0003] The insecticidal mechanism of cartap is that it can penetrate into the junction of nerve cells and block the transmission of acetylcholine secreted by one cell to the second nerve cell. Therefore, it is the opposite of organophosphorus pesticides. It makes the nerve cells of the insect body neither excite normally, nor transmit and stimulate the second nerve cells, lose the ability to eat and damage crops, stop developm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C333/04
CPCC07C333/04
Inventor 邹从伟戴久坤周芬沈永刚
Owner 仪征市海帆化工有限公司
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