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Synthesis method of chloromethyl thiazole

A technology for chloromethylthionitrone and chloromethylthionitrogen, which is applied in the synthesis field of chloromethylthionitrone, can solve problems such as difficult operation, large pollution, complicated procedures, etc., and achieves a high degree of automation and process safety. Controllable and reasonable process design effect

Inactive Publication Date: 2018-09-04
岳阳景嘉化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] In order to overcome the above-mentioned shortcomings, the patent of the present invention provides a new synthesis route of chloromethylthiazocene, which solves the problem that there are many by-products in the synthesis of chloromethylthiazocene at this stage, the yield is low, the process is complicated, the pollution is large, the waste of raw materials is high, and the cost is high. Disadvantages, low purity, difficult temperature control, difficult operation, etc.

Method used

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  • Synthesis method of chloromethyl thiazole
  • Synthesis method of chloromethyl thiazole

Examples

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Effect test

Embodiment 1-4

[0045] Example 1-4: Synthesis of 1-isothiocyanato-2-chloro-2-propene:

Embodiment 1

[0046]Example 1: 150g of 2,3-dichloropropene, 108g of sodium thiocyanate, and 150g of dichloromethane were added to a 500ml three-necked flask, and the spherical condenser was passed through a 0-5 degree ice salt water, heated in a water bath, slightly refluxed, and refluxed for 3 reactions After 2 hours, the content of 2,3-dichloropropene was detected to be lower than 0.2%, and the material was cooled to below 10 degrees with ice brine, filtered, and the filter cake was washed with 150 g of dichloromethane to combine the mother liquor for the next step of synthesis. The content of the product 1-isothiocyanato-2-chloro-2-propene was >99.5%, and the internal standard of the product was used to obtain 180 g of the product 1-isothiocyanato-2-chloro-2-propene, with a yield of 99.5%.

Embodiment 2

[0047] Example 2: In a 500ml three-necked flask, add 150g of water and 108g of sodium thiocyanate, stir for 10 minutes to dissolve, add 150g of 2,3-dichloropropene, slowly heat up to 50-60 degrees to react, and the spherical condenser tube is fed with frozen brine, React for 2-3 hours, check the end point, the content of 2,3-dichloropropene is less than 0.2%, then cool the material to below 10 degrees, pour it into a separatory funnel to separate layers, and add sodium to treat the upper layer of saline wastewater. 178 g of 1-isothiocyanato-2-chloro-2-propene in the lower organic phase was collected, with a content of 99.5% and a yield of 98.8%.

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Abstract

The invention discloses a synthesis method of chloromethyl thiazole, and 1-isothiocyano-2-chlorine-2-propylene and chlorine are taken as the raw materials to react to obtain chloromethyl thiazole. Theprocess is simple, the reaction route is short, the cost is low, the yield is high, the molar yield is up to 99% (compared with dichloropropene), the process design is reasonable, the process is safeand controllable, no wastewater process is used, and the cost for treating wastewater is reduced.

Description

technical field [0001] The invention relates to a synthesis method of chloromethylthiazocene, which belongs to the technical field of pharmaceutical intermediates. Background technique [0002] The structural formula of chloromethylthiazole is: Chloromethylthiazol is the latest generation of basic pharmaceutical raw materials in the world, and it is a special drug raw material for the treatment of depression, asthma and other diseases. The downstream pharmaceutical products of chloromethylthiazepine, serotonin and ipratropine, can be transformed and decomposed in the body and excreted in urine. So it has the characteristics of high efficiency and low side effects. And its medical effect can be better than monoamine oxidase inhibitors and terbutaline, which are currently ranked huge in annual sales, and the cost is lower than monoamine oxidase inhibitors and terbutaline (annual sales of 1 billion US dollars), it can be expected that Monoamine oxidase inhibitors and terbut...

Claims

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Application Information

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IPC IPC(8): C07D277/32
CPCC07D277/32
Inventor 李伊黾李琼
Owner 岳阳景嘉化工有限公司
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