Synthesis method for organically synthesizing intermediate N-allylthiourea

A technology of acryl urea and organic synthesis, applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problems of low final yield and complicated process, shorten the reaction time and reduce the intermediate links , the effect of increasing the reaction yield

Inactive Publication Date: 2018-08-14
CHENGDU ZHONGHENG HUATIE TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This technology helps reduce intermediates between reactions faster by making them shorter or more efficient.

Problems solved by technology

The technical problem addressed in this patented text relates to finding an improved way to make certain chemicals that are less expensive than traditional ways such as silver nitrate or sulfur dioxide.

Method used

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  • Synthesis method for organically synthesizing intermediate N-allylthiourea

Examples

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Effect test

example 1

[0011] Add 4mol of urea, 3mol of propylene alcohol, 12L of 40% potassium bromide solution, 1.5mol of alumina powder into the reaction vessel, control the stirring speed to 90rpm, increase the solution temperature to 80°C, keep it for 100min, and reduce the pressure at 20kP Distill, lower the solution temperature to 10°C, precipitate crystals, wash with 60% diethyl ether solution and 70% dimethylamine solution, recrystallize in 75% methanol solution, and dehydrate with anhydrous magnesium sulfate agent dehydration, to obtain finished product N-propenyl urea 267g.

example 2

[0013] Add 4.5mol of urea, 3mol of propylene alcohol, 12L of 42% potassium bromide solution, 1.5mol of alumina powder into the reaction vessel, control the stirring speed to 100rpm, increase the solution temperature to 85°C, keep it for 120min, and reduce the temperature at 25kPa. Pressure distillation, lower the solution temperature to 12°C, precipitate crystals, wash with 62% ether solution, 72% dimethylamine solution, recrystallize in 78% methanol solution, dehydrate activated alumina agent dehydration, to obtain 273g of finished product N-propenyl urea.

example 3

[0015] Add 5mol of urea, 3mol of propylene alcohol, 12L of 45% potassium bromide solution, 1.5mol of alumina powder into the reaction vessel, control the stirring speed to 110rpm, raise the solution temperature to 90°C, keep it for 130min, and depressurize at 30kPa Distill, lower the solution temperature to 15°C, precipitate crystals, wash with 65% ether solution, 75% dimethylamine solution, recrystallize in 80% methanol solution, dehydrate with anhydrous magnesium sulfate agent dehydration to obtain 279g of finished product N-propenyl urea.

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Abstract

The invention relates to a synthesis method for organically synthesizing an intermediate N-allylthiourea. The synthesis method mainly comprises: adding 4-5 mol urea, 3 mol allyl alcohol, 12 L of a potassium bromide solution and 1.5 mol alumina powder in a reaction container, controlling the stirring speed at 90-110 rpm, heating the solution to a temperature of 80-90 DEG C, maintaining for 100-130min, carrying out pressure reducing distillation, cooling the solution to a temperature of 10-15 DEG C, precipitating to obtain a crystal, washing with an ether solution, washing with a dimethylaminesolution, re-crystallizing in a methanol solution, and dewatering with a dewatering agent to obtain the finished product N-allylthiourea.

Description

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Claims

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Application Information

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OwnerCHENGDU ZHONGHENG HUATIE TECH CO LTD