Method for synthesizing 5-methyl-5-propyl-1,3-dioxane-2-ketone and carisoprodol
A synthesis method, dioxane technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of carbamic acid derivatives, etc., can solve the problems of high raw material consumption, high cost of raw materials, cumbersome operation, etc., and achieve simplified production Process, reduce energy consumption, improve the effect of utilization
Inactive Publication Date: 2009-07-29
CHONGQING ENSKY CHEM
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Problems solved by technology
[0009] Although the Chinese Patent No. is 200510046686.9, the related work has been improved, but there are still following deficiencies: (1) take diethyl carbonate as raw material to prepare intermediate 5-methyl-5-propyl-1,3-dioxo Hexacyclo-2-one, high raw material cost
(2) Since diethyl carbonate is condensed with 2-methyl-2-propyl-1,3-propanediol, ethanol is produced in the condensation reaction, and it needs to be separated by toluene azeotrope by distillation first in the production process , which not only causes complicated process and cumbersome operation, but also increases energy consumption
(3) When ethanol is separated, a small amount of raw material diethyl carbonate will be steamed out, resulting in high raw material consumption
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[0031] The present invention will be further described below in conjunction with specific embodiments, so as to help understand the content of the present invention.
[0032] 1, the preparation of 5-methyl-5-propyl-1,3-dioxane-2-one (compound II)
[0033] It can be prepared by non-solvent and solvent-based processes.
[0034] (1) Non-solvent preparation
[0035] Add 264 grams of 2-methyl-2-propyl-1,3-propanediol in the reaction flask, 8.1 grams of zinc oxide and 60 grams of urea that have been activated by burning for 2 hours at 450 ° C, and heat up to 110 ° C. The reaction was continued with stirring at low temperature until almost no ammonia gas was released. The released ammonia gas is received by the receiving device. After the reaction was completed, the product 5-methyl-5-propyl-1,3-dioxane-2-one (compound II) was distilled out under reduced pressure to obtain 139 grams. The distillation temperature was 150-160° C. and the pressure was 15 -20mmHg. The calculated yie...
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Abstract
The invention discloses a synthetic method for 5-methyl-5-propyl-1, 3-dioxane-2-ketone and carisoprodol, which uses 2-methyl-2-propyl-1, 3-propanediol as an original material, and the 5-methyl-5-propyl-1,3-dioxane-2-ketone can be generated through a condensation reaction with urea under the catalysis of activated metal oxide; the obtained 5-methyl-5-propyl-1, 3-dioxane-2-ketone is ammonolyzed with isopropylamine, and 2-methyl-2-ethyl-3-hydroxypropyl-N-isopropylcarbamate can be prepared; the 2-methyl-2-ethyl-3-hydroxypropyl-N-isopropylcarbamate reacts with sodium cyanate, and the carisoprodol is prepared. The synthetic method for the 5-methyl-5-propyl-1, 3-dioxane-2-ketone and the carisoprodol is cheap and easily available in raw material, simple in preparation technology and more economical.
Description
technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for synthesizing carisoprodol and its intermediate 5-methyl-5-propyl-1,3-dioxane-2-one. Background technique [0002] Carisoprodol is the most widely used skeletal muscle relaxant drug, and its compound preparation is widely used in the clinical treatment of pain in Europe and the United States, and has received very high evaluations from doctors and patients; Great usage needs. [0003] There are currently two processes for the synthesis of carisoprodol: [0004] (1) Phosgene route [0005] It is phosgenated by 2-methyl-2-propyl-1,3-propanediol, reacted with isopropylamine, then phosgenated again, and ammoniated; domestic routes also use 2-methyl-2-propyl - 1,3-propanediol reacts with triphosgene to generate cyclic carbonate, aminolysis, and sodium cyanate to obtain the crude product of carisoprodol. [0006] This route uses phosgene and solid phosgene, a substit...
Claims
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IPC IPC(8): C07D319/04C07C271/12C07C269/00
Inventor 张毅黄玉明曹原吴明亮
Owner CHONGQING ENSKY CHEM