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Method for compounding drug intermediate allylthiourea

A technology of propylene-based thiourea and a synthesis method, applied in directions such as organic chemistry, can solve problems such as low final yield and complicated process, and achieve the effects of shortening reaction time, reducing intermediate links and improving reaction yield

Inactive Publication Date: 2018-07-10
CHENGDU DONG DIAN AI ER TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the existing synthetic methods use sodium thiocyanate as the reactant, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method, which is helpful for further improving the quality and yield of the product. rate, reducing the content of by-products has important economic significance

Method used

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  • Method for compounding drug intermediate allylthiourea

Examples

Experimental program
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Effect test

example 1

[0011] Add 5L mass fraction of 10% sodium chloride solution, 4mol of 3-methylisothiocyanate benzene in the reaction vessel, increase the solution temperature to 60°C, add 5mol of allylamine and 6L of 15% acetone solution , reflux for 90min, stand to separate layers, take out the oil layer, wash 5 times with potassium bromide solution to obtain propylene isothiocyanate, dehydrate with dehydrating agent, filter, distill the filtrate under reduced pressure at 20kPa, collect the fraction at 80°C to obtain thiocyanate Propyl thiocyanate; add the obtained propylene thiocyanate to 5mol phenylacetamide, add 2L aqueous solution, raise the temperature of the solution to 50°C, react for 50min, lower the temperature of the solution to 10°C, precipitate crystals, filter, and the mass fraction is 70 % toluene solution, 85% butanone solution by mass fraction, and dehydration with anhydrous potassium carbonate dehydrating agent to obtain 408.32 g of finished product propenylthiourea, with a yi...

example 2

[0013] Add 5L mass fraction of 13% sodium chloride solution, 4mol of 3-methylisothiocyanate benzene in the reaction vessel, increase the solution temperature to 62°C, add 5.5mol of allylamine and 6L of 17% acetone Solution, reflux for 110min, stand to separate layers, take out the oil layer, wash 6 times with potassium bromide solution to obtain propylene isothiocyanate, dehydrate with a dehydrating agent, filter, and distill the filtrate under reduced pressure at 25kPa, collect the fraction at 83°C to obtain sulfur Propylene cyanate; add the obtained propenyl thiocyanate to 5.5mol phenylacetamide, add 2L aqueous solution, raise the solution temperature to 55°C, react for 60min, lower the solution temperature to 12°C, precipitate crystals, filter, mass fraction Wash with 75% toluene solution, wash with 87% butanone solution by mass fraction, and dehydrate with anhydrous calcium sulfate dehydrating agent to obtain 426.88 g of finished allylthiourea with a yield of 92%.

example 3

[0015] Add 5L mass fraction of 16% sodium chloride solution, 4mol of 3-methylisothiocyanate benzene in the reaction vessel, increase the solution temperature to 65°C, add 6mol of allylamine and 6L of 20% acetone solution , reflux for 120min, stand for stratification, take out the oil layer, wash 7 times with potassium bromide solution to obtain propylene isothiocyanate, dehydrate with a dehydrating agent, filter, and distill the filtrate under reduced pressure at 30kPa, collect the fraction at 86°C to obtain thiocyanate Propyl thiocyanate; add the obtained propylene thiocyanate to 6mol phenylacetamide, add 2L aqueous solution, raise the temperature of the solution to 60°C, react for 70min, lower the temperature of the solution to 15°C, precipitate crystals, filter, and the mass fraction is 80 % toluene solution, washing with 90% butanone solution by mass fraction, and dehydration with anhydrous potassium carbonate dehydrating agent to obtain 436.16 g of finished allylthiourea, ...

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Abstract

The invention provides a method for compounding drug intermediate allylthiourea. The method mainly comprises the following steps that 5 liters of sodium chloride solution and 4 moles of 3-methyl isothiocyanate benzene are added into a reaction vessel, the temperature of the solution is heated to 60-65 DEG C, 5-6 moles of allylamine and 6 liters of acetone solution are added into, then circulationreflux is carried out for 90-120 minutes, standing stratification is carried out, an oil layer is taken out, washing is carried out for 5-7 times through a potassium bromide solution to obtain allyl isothiocyanate, dehydration is carried out through a dehydrating agent, filtering is carried out, reduced pressure distillation is carried out on a filter liquid cut fraction of 80-86 DEG C is collected to obtain allyl rhodanate; the obtained allyl rhodanate is added into 5-6 moles of phenylacetamide, 2 liters of water solution is added into, the temperature of the solution is heated to 50-60 DEG C, reaction is carried out for 50-70 minutes, the temperature of the solution is reduced to 10-15 DEG C, crystal precipitation is carried out, filtering is carried out, washing is carried out by a methylbenzene solution and a butanone solution in sequence, and dehydration is carried out through a dehydrating agent to obtain finished allylthiourea.

Description

technical field [0001] The invention relates to a method for synthesizing a pharmaceutical intermediate, propenylthiourea. Background technique [0002] Propylthiourea is mainly used as antiseptic, topical medicine, plastic surgery, scar removal, cosmetics, skin micro-scar removal; cyanide-free copper plating additive; organic synthesis raw material. It is used to inhibit nitrification reaction in sewage test. However, most of the existing synthetic methods use sodium thiocyanate as the reactant, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method, which is helpful for further improving the quality and yield of the product. It is of great economic significance to reduce the content of by-products. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of medicine intermediate allyl thiourea, comprises the steps: [0004] (i) Add 5L of ...

Claims

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Application Information

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IPC IPC(8): C07C335/10
CPCC07C335/10C07C331/04
Inventor 严义达
Owner CHENGDU DONG DIAN AI ER TECH
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