IES87001B2

IES87001B2 - Organic synthesis intermediates N-propenyl urea synthesis method

Info

Publication number: IES87001B2
Application number: IES20180102A
Authority: IE
Inventors: Peng Xiangliang
Original assignee: Chengdu Zhong Heng Hua Tie Tech Co Ltd
Priority date: 2018-04-03
Filing date: 2018-04-03
Publication date: 2019-05-01
Also published as: IES20180102A2

Abstract

Organic synthesis intermediates N-propenyl urea synthesis method, comprises the following steps: adding 4-5 mol allyl alcohol, 12 L potassium bromide solution, 1.5 mol alumina powder, controlling the stirring speed at 90-110rpm, raising the temperature of the solution to 80-90 °C, keeping the temperature for 100-130min, then distilled it under reduced pressure, reducing the solution temperature to 10-15°C, precipitated crystals, washed with ether solution, and dimethylamine solution, recrystallized in methanol solution, the dehydrated with dehydrating agent to obtain the finished product.

Description

Organic synthesis intermediates N-propenyl urea synthesis method FIELD OF THE INVENTION The present invention relates to organic synthesis intermediates N-propeny! urea synthesis method.

GENERAL BACKGROUND N-propylene urea is mainly used for non-cyanide copper additives, preservatives, organic synthesis of raw materials, however, most of the existing synthetic methods are complicated and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method for further improving the quality and yield of the product and reducing the byproduct content, it has important economic significance.

SUMMARY The purpose of the present invention is to provide organic synthesis intermediates N-propenyl urea synthesis method, comprises the following steps: (i) adding 4-5 mol urea, 3 mol allyl alcohol, 12 L potassium bromide solution, 1.5mol alumina powder, controlling the stirring speed at 90-110rpm, raising the temperature of the solution to 80-90”C, keeping the temperature for 100-130min, then distilled it under reduced pressure, reducing the solution temperature to 10-15°C, precipitated crystals, washed with ether solution, and dimethylamine solution, recrystallized in methanol solution, the dehydrated with dehydrating agent to obtain the finished product; wherein, potassium bromide solution in step (i) has a mass fraction of 40-45%; the pressure of the vacuum distillation in step (i) is 20-30kPa, the mass fraction of the ether solution in the step (i) is 60-65%, the dimethylamine solution in the step (i) has a mass fraction of 70-75%, the methanol solution in the step (i) has a mass fraction of 75-80%, the dehydrating agent in the step (i) is any one of anhydrous magnesium sulfate and activity alumina.

Throughout the reaction process can be the following reaction formula: CH2 HC 'CH, OH KBi -----SwCHS II HC.

CH, I UN Advantage of the present invention is that: reducing intermediate links reaction, decreasing the reaction time and improving the reaction yield.

DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS The following examples with reference to specific embodiments of the present invention are further illustrated: organic synthesis intermediates N-propenyl urea synthesis method.

Embodiment 1 mol urea, 3 mol allyl alcohol, 12 L potassium bromide solution with a mass fraction of 40% and 1.5 mol alumina powder were added to the reaction vessel, the stirring speed is controlled to 90 rpm and the temperature of the solution is raised to 80 °C for 100 min, distilled it under reduced pressure of 20kP, reducing the solution temperature to 10 °C, precipitated crystals, washed with diethyl ether solution with a mass fraction of 60%, and with dimethylamine solution with a mass fraction of 70%, recrystallized in 75% methanol solution, dehydrated with magnesium sulfate dehydrating agent to obtain the finished product N-propenyl urea 267g.

Embodiment 2 4.5mol urea. 3mol allyl alcohol, 12L potassium bromide solution with a mass fraction of 42% and 1.5mol alumina powder were added into the reaction vessel, the stirring speed was controlled at lOOrpm, the temperature of the solution is raised to 85 °C for 120min, distilled it under reduced pressure of 25kPa, reducing the solution temperature to I2“C, precipitated crystals, washed with ethyl ether solution with a mass fraction of 62%, dimethylamine solution with a mass fraction of 72%, recrystallized in methanol solution with a mass fraction of 78%, and dehydrated with activated alumina dehydrating agent, to obtain the finished product N-propenyl urea 5 273g.

Embodiment 3 5mol urea, 3mol allyl alcohol, 12L potassium bromide solution with a mass fraction of 45% and 1.5mol alumina powder were added into the reaction vessel, the 0 stirring speed was controlled at llOrpm and the temperature the solution was increased to 90°C for 130min and distilled it under reduced pressure of 30kPa, the solution is cooled to 15 °C, the precipitated crystals were washed with ethyl ether solution with a mass fraction of 65% and dimethylamine solution with a mass fraction of 75%, recrystallized in methanol solution with a mass fraction of in 80% methanol 5 solution, and dehydrated with magnesium sulfate dehydrating agent to obtain the finished product N-propylene urea 279g.

Claims

1. Organic synthesis intermediates N-propenyl urea synthesis method, comprises the following steps: (i) adding 4-5 mol urea, 3 mol allyl alcohol, 12 L potassium bromide solution, 1.5 mol alumina powder, controlling the stirring speed at 90-110rpm, raising the temperature ofthe solution to 80-90°C, keeping the temperature for 100-130min, then distilled it under reduced pressure, reducing the solution temperature to 10-15°C, precipitated crystals, washed with ether solution, and dimethylamine solution, recrystallized in methanol solution, the dehydrated with dehydrating agent to obtain the finished product; wherein, potassium bromide solution in step (i) has a mass fraction of 40-45%; the pressure ofthe vacuum distillation in step (i) is 20-30kPa, the mass fraction of the ether solution in the step (i) is 60-65%, the dimethylamine solution in the step (i) has a mass fraction of 70-75%.

2. Organic synthesis intermediates N-propenyl urea synthesis method according to claim 1 wherein the methanol solution in the step (i) has a mass fraction of 75-80%.

3. Organic synthesis intermediates N-propenyl urea synthesis method according to claim 1 wherein the. dehydrating agent in the step (i) is any one of anhydrous magnesium sulfate and activity alumina.