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Preparation method of (R)-propylene carbonate

A technology of propylene carbonate and acetic acid, which is applied in the direction of organic chemistry, can solve the problems of high production risk, high equipment requirements, and low yield, and achieve the effects of reduced production cost, high product yield, and high utilization rate

Inactive Publication Date: 2015-01-14
扬州三友合成化工有限公司
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Problems solved by technology

This method requires high equipment, high production risk and low yield

Method used

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  • Preparation method of (R)-propylene carbonate

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Embodiment Construction

[0019] 1. Preparation of (R)-1,2-propanediol:

[0020] Weigh 0.002 mol (0.833g) of (S, S)-Salen Co catalyst into a 100 mL flask, add 18.4ml of toluene, then add 14.5mmol (0.87g) of AcOH, and then open to air and stir for 0.5h Activation of the catalyst. It can be seen that the reaction system gradually changes from brick red to dark brown, that is, the catalyst is activated. The toluene was then removed with a vacuum pump, leaving a dark brown solid, the activated catalyst.

[0021] Mix 40g of propylene oxide and 0.002mol of the activated catalyst in a flask, place the mixed system in an ice bath to 0-5°C, and slowly add 5.6g of water dropwise at the same time, then remove the ice bath, and then stir the reaction at room temperature 14 h. After the reaction, (S)-propylene oxide was distilled out under normal pressure, and then vacuum distillation was carried out with an oil pump to obtain 25.6 g of (R)-1,2 propanediol with a yield of 98%.

[0022] 2. Preparation of (R)-pro...

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Abstract

The invention relates to a preparation method of (R)-propylene carbonate and belongs to the technical field of medicine production and the technical field of preparation of a tenofovir intermediate particularly. The preparation method comprises the following steps of: activating a catalyst by adopting methylbenzene and acetic acid in air; mixing epoxy propane and the activated catalyst, then dropwise adding water, then stirring to react under the condition of normal temperature, then distilling out (S)-epoxy propane, and then carrying out reduced pressure distillation to obtain (R)-1,2-propanediol; mixing (R)-1,2-propanediol, carbamide and zinc oxide, reacting till the end under the condition of environmental temperature of 100-120 DEG C, then carrying out the reduced pressure distillation to remove (R)-1,2-propanediol, and then continuously distilling to obtain the (R)-propylene carbonate. The preparation method disclosed by the invention is low in production cost. According to the preparation method, the excessive (R)-1,2-propanediol is recovered to be continuously used, and the used raw material urea is more favorable to clean production in comparison with diethyl carbonate.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical production, in particular to the technical field of preparation of tenofovir intermediates, in particular to a preparation method of (R)-propylene carbonate. Background technique [0002] (R)-Propylene carbonate is a key intermediate in the synthesis of anti-AIDS and anti-hepatitis B virus drug Tenofovir (Tenofovir). In recent years, the following two methods have been used to produce (R)-propylene carbonate at home and abroad. [0003] The first method: obtain (R)-1,2-propanediol from racemic propylene oxide by hydrolysis resolution, and then react with dimethyl carbonate or diethyl carbonate to produce the product. The methanol and dimethyl carbonate or ethanol and diethyl carbonate produced in this method will all be azeotropic and should not be separated, so the raw materials will not be fully utilized and the cost of raw materials will be high (see "R by Ding Huaping, Chen Yu, Jixiang...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/36
CPCC07D317/36
Inventor 张扬李明成李辉宁张众笑张才山
Owner 扬州三友合成化工有限公司
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