Synthesis method of ethyl 2-methylpyrimidyl-4-carboxylate
A technology of methyl pyrimidine and ethyl carboxylate, which is applied in the field of medicine and can solve problems such as failure to obtain target products
Inactive Publication Date: 2012-09-19
CGENETECH (SUZHOU CHINA) CO LTD
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However, the above-mentioned processes failed to obtain the target product under conventional laboratory conditions, so the existing synthetic method was obtained by modifying the synthetic route
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[0014] The synthetic method of described ethyl 2-methylpyrimidine-4-carboxylate is obtained: take 7.2 g vinyl ethyl ether, 9.48 g pyridine, after cooling to zero, slowly add 16.4 g monoethyl oxalyl chloride dropwise, dropwise Afterwards, keep the same temperature, continue stirring for 10 min, and the system rises to room temperature and stirs overnight. The next day, it was directly purified on a packed silica gel column to obtain 16.43 g. 5-ethoxy-4-ene-oxalic acid monoethyl ester, then reflux with acetamidine acetate and potassium carbonate in ethanol overnight, filter the next day, spin dry and pass through the column to obtain 2-methylpyrimidine-4-carboxylic acid ethyl ester 8g.
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The invention discloses a synthesis method of ethyl 2-methylpyrimidyl-4-carboxylate. According to the existing documents, the target product can not be obtained through many trials by using 2-bromopyrimidine and diethyl malonate or ethyl 3-oxyethyl-2-methacrylate and acetamidine acetate as raw materials. The invention optimizes the synthesis route to obtain the method for synthesizing the ethyl 2-methylpyrimidyl-4-carboxylate. The invention mainly improves the synthesis method of ethyl 2-methylpyrimidyl-4-carboxylate, lowers the strict requirements for reaction conditions, and simplifies the operation.
Description
technical field [0001] The invention relates to a synthesis process method of ethyl 2-methylpyrimidine-4-carboxylate, which belongs to the technical fields of medicine and chemical industry. Background technique [0002] Ethyl 2-methylpyrimidine-4-carboxylate is a white solid and is an important pharmaceutical intermediate. [0003] The synthetic technique of existing 2-methylpyrimidine-4-ethyl carboxylate is to adopt 3-ethoxy-2-ethyl methacrylate, and 2-bromopyrimidine and diethyl malonate as raw materials, React with acetamidine acetate to obtain ethyl 2-methylpyrimidine-4-carboxylate. However, none of the above processes could obtain the target product under normal laboratory conditions, so the existing synthetic method was obtained by modifying the synthetic route. Contents of the invention [0004] In view of the unfeasibility of the original two methods, the present invention finally determines the process route of this patent after trying a route on the premise of...
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IPC IPC(8): C07D239/28
Inventor 徐余冬丁炬平张仁延余强
Owner CGENETECH (SUZHOU CHINA) CO LTD