- High-purity 5-ethyl-5-(1-methylbutyl)barbituric acid preparation method
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The present invention relates to a preparation method of a drug pentobarbital (1) for sedation, hypnosis, pre-anesthesia administration and anti-convulsion, and provides a new preparation process for preparing high-purity pentobarbital (I) from diethyl ethylmalonate, wherein the process comprises three steps: A, bromination; B, alkylation; and C, cyclization, acidification, and purification. According to the present invention, the method has advantages of simple operation, short production cycle, low energy consumption, mother liquor circulation, less three-waste, stable process, good product quality, high product purity, isomer impurity content of less than 0.1%, high yield and low production cost, and is suitable for industrial production.
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Paragraph 0021; 0024; 0025; 0028; 0029; 0032; 0033; 0036
(2019/10/04)
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- 5-ethyl-5 - (1-methyl butyl) method for preparing malonyl urea (by machine translation)
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The invention belongs to the technical field of drug synthesis, in particular relates to a 5-ethyl-5 - (1-methyl butyl) method for preparing malonyl urea. Ethyl malonic acid diethyl ester (III) with ethanol after the reaction ethanol solution of sodium in toluene in the presence of a mixture of the methanesulfonic acid (2-pentyl) should be ester instead, rectification to get ethyl-(1-methyl butyl) malonic acid diethyl ester compound (II); compound (II) in the presence of a methanol solution of sodium methoxide reaction with urea, acidified by hydrochloric acid, is recrystallized to get 5-ethyl-5 - (1-methyl butyl) malonyl urea fine (I). The process of the invention is stable, mild reaction conditions, is easy to control, the resulting product has high purity, high yield, the conversion is almost 100%, after treatment is simple and convenient, low energy consumption, little three waste, the mother liquor can be used continuously, low production cost, is suitable for industrial production. (by machine translation)
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Paragraph 0030; 0031
(2016/12/12)
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