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Method for preparing oxiracetam

A chloroacetoacetate and pressure technology, applied in the field of chemical raw material preparation, can solve problems such as high yield and short steps, and achieve the effects of improving reaction yield, fast reaction speed, and increasing effective collision probability

Inactive Publication Date: 2012-08-15
SHIJIAZHUANG LICKON PHARMATECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the shortcomings of the existing oxiracetam preparation method, provide an environmental protection, short steps, high yield, and be beneficial to the method for preparing oxiracetam in industrialized production

Method used

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  • Method for preparing oxiracetam
  • Method for preparing oxiracetam
  • Method for preparing oxiracetam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take a mixture of 49.38g (300mmol) ethyl 4-chloroacetoacetate and 100ml ethanol and pour it into a 200ml single-necked bottle, and degas it with ultrasonic waves under reduced pressure. Quickly weigh 10.64mg (0.06mmol) of palladium chloride and 29.9mg (0.06mmol) of DIOP ligand with a microbalance, and then add them, degassed substrate and solvent into a 500ml autoclave under nitrogen protection. At room temperature, the air in the autoclave was replaced with nitrogen, then replaced with hydrogen three times, and filled with hydrogen to the pressure required for the reaction. Allow it to react at the set temperature for a certain period of time until the pressure does not change and stop the reaction. Pass circulating water to cool the temperature of the kettle body to room temperature, release hydrogen carefully, take out the reactor, evaporate the solvent on a rotary evaporator, and finally use an oil pump to distill under reduced pressure at 15 mm Hg and collect the f...

Embodiment 2

[0030] Take a mixture of 45.18g (300mmol) methyl 4-chloroacetoacetate and 100ml methanol and pour it into a 200ml single-necked bottle, and use ultrasonic degassing under reduced pressure. Quickly weigh 10.64mg (0.06mmol) of palladium chloride and 29.9mg (0.06mmol) of DIOP ligand with a microbalance, and then add them, degassed substrate and solvent into a 500ml autoclave under nitrogen protection. At room temperature, the air in the autoclave was replaced with nitrogen, then replaced with hydrogen three times, and filled with hydrogen to the pressure required for the reaction. Allow it to react at the set temperature for a certain period of time until the pressure does not change and stop the reaction. Pass circulating water to cool the temperature of the kettle body to room temperature, release hydrogen carefully, take out the reactor, evaporate the solvent on a rotary evaporator, and finally use an oil pump to distill under reduced pressure at 15 mm Hg and collect the fract...

Embodiment 3

[0033] Take a mixture of 49.38g (300mmol) ethyl 4-chloroacetoacetate and 100ml methanol and pour it into a 200ml single-necked bottle, and use ultrasonic degassing under reduced pressure. Quickly weigh 12.56mg (0.06mmol) of rhodium trichloride and 27.51mg (0.06mmol) of the DIPAMP ligand with a microbalance, then add it and degassed substrate and solvent to a 500ml autoclave under nitrogen protection . At room temperature, the air in the autoclave was replaced with nitrogen, then replaced with hydrogen three times, and filled with hydrogen to the pressure required for the reaction. Allow it to react at the set temperature for a certain period of time until the pressure does not change and stop the reaction. Pass circulating water to cool the temperature of the kettle body to room temperature, carefully release hydrogen, take out the reactor, evaporate the solvent on a rotary evaporator, and finally use an oil pump to distill under reduced pressure at 6 mm Hg and collect the fr...

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Abstract

The invention discloses a method for preparing oxiracetam. The method comprises the following step of carrying out catalytic hydrogenation by taking 4-chloro-acetylacetic ester as a raw material under the action of certain temperature, certain pressure and a catalyst to obtain 4-cholor-3-hydroxyl butyrate. According to the method, three wastes can be avoided, the environmental pollution can be avoided, the raw material 4-chloro-acetylacetic ester is low in price and easy to obtain, the yield is high, and a product can be almost quantitatively obtained. A microwave reaction method is used in the step of preparing the oxiracetam by cyclization, so that the unnecessary loss of heat energy can be reduced, the reaction yield and the reaction rate are improved, and the product is easy to separate and purify.

Description

technical field [0001] The invention relates to a method for preparing oxiracetam, which belongs to the technical field of preparation of chemical raw materials. Background technique [0002] Oxiracetam, its chemical name is 4-hydroxypyrrolidone-2-acetamide, and its chemical structure is as follows: [0003] [0004] It is a new generation of drug for improving brain metabolism. It is a derivative of pyrrolidone (cyclic GABOB) and an analogue of piracetam. All have good curative effect. Oxiracetam was first produced and marketed in Europe by the Italian company ISFS.S.P.A in 1987, and is now on the market in 40 countries and regions around the world. There have been a lot of reports on the synthesis of oxiracetam over the years. Patents US5276164; US4118396; JP9026267; CN101121688 report that diketene is used as a starting material to obtain oxiracetam through different routes, but the common problem of this method is that the reaction steps are long and the yield is l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/273C07C69/72
Inventor 刘庆彬李耀锋温海山刘海兰李立斌靳晓坤
Owner SHIJIAZHUANG LICKON PHARMATECH
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