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Preparation method of cartap hydrochloride intermediate, i.e., 2-N, N-dimethyl-1, 3-dithio-cyano propane

A technology of dithiocyanopropane and dimethyl, which is applied in the field of thiocyanate intermediate 2-N, can solve the problems of low thiocyanate yield, high processing cost, poor working environment and the like, and achieves convenient process implementation, The effect of high yield of normal isomer and less amount of three wastes

Active Publication Date: 2009-09-02
ZHEJIANG BOSHIDA CROP TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, during the preparation of rhodanide, in the process of separating and washing the highly toxic sodium cyanide reaction solution, not only the working environment is poor, the risk of poisoning is high, but also a large amount of cyanide-containing wastewater is produced, and the treatment cost is high.
CN1060913C, invention title "preparation method of cartap", discloses an improved method for preparing cartap from raw materials such as insecticide, sodium cyanide, methanol, hydrogen chloride gas, etc., although the operation has been improved, but still did not avoid the use of highly toxic sodium cyanide raw materials
Adopt non-cyanide route to synthesize thiocyanide, inevitably produce more thiocyanide isomers, though can improve the orthomer content of thiocyanide by changing reaction conditions such as: reduce reaction temperature and other measures, but thiocyanide The yield of thiocyanide will be lower, and the content of thiocyanide can not reach the requirement of making high-content cartap, so the product has no industrial significance

Method used

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  • Preparation method of cartap hydrochloride intermediate, i.e., 2-N, N-dimethyl-1, 3-dithio-cyano propane
  • Preparation method of cartap hydrochloride intermediate, i.e., 2-N, N-dimethyl-1, 3-dithio-cyano propane
  • Preparation method of cartap hydrochloride intermediate, i.e., 2-N, N-dimethyl-1, 3-dithio-cyano propane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Put 400g of n-butanol, 115g of sodium thiocyanate, and 110g of 1-N,N-dimethyl-2,3-dichloropropylamine with a content of 95% into the reaction flask. Any value can be selected within the range of 45~85℃, including the end value), heat preservation reaction for 5 hours, the ratio of thiocyanide normal and isomer: normal structure 51%, isomer 48%, filter out the chlorination Sodium inorganic salt, the filtrate cooled to precipitate crystals, filtered to obtain thiocyanide isomer solid crystals (normal form 5%, isomer 94%), dried 57g, the filtrate was frozen and crystallized, filtered to obtain thiocyanide normal form ( The normal form is 97%, the isomer is 2%), 54g is dry, and the yield of the normal form of thiocyanide is 39%.

Embodiment 2

[0023] Example 2: Put 400g of n-butanol into the reaction flask, 57g of the isomer obtained in Example 1, 58g of sodium thiocyanate, 55g of 95% 1-N,N-dimethyl-2,3-dichloride Propylamine, heat up 45~85℃ (any value can be selected within the range of 45~85℃, including the end value), heat preservation reaction for 5 hours, the ratio of normal and isomer of thiocyanide, normal body 51%, isomer 47 %, filtered to remove the sodium chloride inorganic salt generated, the filtrate was cooled to precipitate crystals, and filtered to obtain solid crystals of thiocyanide isomers (normal structure 6%, isomer 93%), dried 58g, and the filtrate was frozen and crystallized. The normal form of thiocyanide (98% of normal form and 1% of isomer) was obtained by filtration, which was 53 g in dry form. The yield of normal form of thiocyanide was 77%.

Embodiment 3

[0024] Example 3: Put 500g of acetone into the reaction flask, 58g of the isomer obtained in Example 2, 58g of sodium thiocyanate, 55g of 1-N,N-dimethyl-2,3-dichloropropylamine with a content of 95%, The temperature is increased to 45~70℃ (any value can be selected within the range of 45~70℃ and the end value is included), and the reaction is kept for 5 hours. The ratio of normal thiocyanide to isomer is 50% for normal isomer and 48% for isomer. The inorganic salt of sodium chloride was filtered off, the filtrate was cooled to precipitate crystals, and the solid crystals of thiocyanide isomers were obtained by filtration (normal form 5%, isomer 94%), which was dried 58g, the filtrate was frozen and crystallized, and filtered to obtain The normal form of thiocyanide (98% of normal form, 1% of isomer), 52g in dry form, the yield of normal form of thiocyanide is 76%.

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Abstract

The invention relates to a preparation method for cartap hydrochloride intermediate, i.e., 2-N, N-dimethyl-1, 3-dithio-cyano propane, which takes 1-N, N-dimethyl-2, 3- propylamine dihalide, thiocyanate as the raw material, obtains the mixture of 2-N, N-dimethyl-1, 3-dithio-cyano propane and 3-N, N-dimethyl-1, 2-dithio-cyano propane by reaction with the existence of a solvent, and obtains 2-N, N-dimethyl-1, 3-dithio-cyano propane with high content by separation; simultaneously, 3-N, N-dimethyl-1, 2-dithio-cyano propane isomer participates the reaction circularly, thus having high yield, good product quality, small amount of three wastes, and better industrial application prospect.

Description

Technical field [0001] The invention relates to a method for preparing 2-N,N-dimethyl-1,3-dithiocyanopropane, an intermediate of Shadandan. technical background [0002] 2-N,N-Dimethyl-1,3-dithiocyanopropane (thiocyanide for short) is an essential intermediate for the preparation of the insecticide carbamoylthio derivatives, US3332943, the name of the invention "carbamoylthio derivatives", which is related to carbamoylthio derivatives. The method for preparing salidan from the intermediate thiocyanate of salidan, and involves the normal form and isomer of the intermediate thiocyanide, and the corresponding salidan with the normal structure and the isomer of salidan after hydrolysis, the structural formula is as follows : [0003] [0004] Formula A: 2-N,N-Dimethyl-1,3-dithiocyanopropane (thiocyanide normal structure); Formula B: Salamant normal structure [0005] [0006] Formula C: 3-N,N-dimethyl-1,2-dithiocyanopropane (thiocyanide isomer) [0007] Formula D: Shazadan isomer...

Claims

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Application Information

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IPC IPC(8): C07C331/12C07C333/04
Inventor 沈新良吴华龙徐黎婷
Owner ZHEJIANG BOSHIDA CROP TECH CO LTD
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