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Preparation method of amfebutamone intermediate m-chlorophenylacetone

A technology of chloropropiophenone and bupropion, applied in the field of medicine, can solve the problems of potential safety hazards, low reaction selectivity, etc., and achieve the effects of reducing damage, good catalytic activity, and controlling production costs

Inactive Publication Date: 2013-10-23
WEIHAI DISU PHARMA CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0023] The reaction selectivity of this method is not high, and the generated ketone group is very easy to further react with the Grignard reagent to obtain a by-product tertiary alcohol; and because the acid chloride and the Grignard reagent will decompose and fail when they meet water, the reaction solvent must be dehydrated processing; ether is used as a solvent in the process, ether is extremely flammable, and there are obvious potential safety hazards in industrial production

Method used

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  • Preparation method of amfebutamone intermediate m-chlorophenylacetone
  • Preparation method of amfebutamone intermediate m-chlorophenylacetone
  • Preparation method of amfebutamone intermediate m-chlorophenylacetone

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Embodiment 1

[0033] Add 100 kg of propiophenone into the reaction kettle, add 150 kg of anhydrous aluminum trichloride in 5 batches under slow stirring, and control the temperature at 20-25°C during the feeding process. After the completion of the feeding of aluminum trichloride, continue to insulate and stir for 0.5 hour to make the system uniform. Start to heat up, and when the temperature is 70°C, start to feed chlorine gas, and control the chlorine gas feed rate to 9kg / h. When the amount of feed reaches 55kg, HPLC will follow up and detect the reaction. When the remaining amount of propiophenone is less than 1.0%, stop feeding chlorine gas. The time of feeding chlorine gas is 6 hours, and the amount of chlorine gas is 60kg; cool to room temperature, and pour the reaction solution into 300kg In the crushed ice solution of hydrochloric acid, let stand to separate layers, remove the water phase, wash the organic phase with water, collect all fractions by distillation under reduced pressur...

Embodiment 2

[0035] Add 200kg of propiophenone into the reaction kettle, add 400kg of anhydrous aluminum trichloride in 6 batches under slow stirring, control the temperature not to exceed 25°C, continue to keep warm and stir for 1 hour after feeding the aluminum trichloride to make the system uniform. Slowly raise the temperature. When the temperature rises to 80°C, start to feed chlorine gas, and control the chlorine gas feed rate to 23kg / h. When the gas flow reaches 116kg, HPLC will track and detect the reaction. When the remaining amount of propiophenone is less than 1.0%, stop feeding Chlorine, the chlorine gas time is 5 hours. The amount of chlorine used is 136kg; cooled to room temperature, the reaction solution is poured into 800kg hydrochloric acid crushed ice solution, allowed to stand for stratification, the water phase is removed, the organic phase is washed with water, the pressure is 400Pa, and the temperature is reduced pressure distillation at 135°C to collect all Distillat...

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Abstract

The invention is mainly aimed at providing a preparation method of amfebutamone intermediate m-chlorophenylacetone. According to the preparation method, a chlorination reaction is carried out on propiophenone serving as raw material to prepare m-chlorophenylacetone in one step, wherein anhydrous aluminum chloride is used as a catalyst in the reaction and has the advantages of good catalytic activity and high reaction selectivity; the whole reaction is simple in operation steps and mild in conditions; the adopted raw material propiophenone, aluminum chloride and chlorine gas are cheap and easily available, so that the production cost can be well controlled; no organic solvent is used in the reaction, thereby reducing injury to operators, decreasing atmospheric environmental pollution and meeting the demands of environmentally-friendly catalyzed synthesis, energy saving and emission reduction; and the purity of the m-chlorophenylacetone prepared by the invention can be higher than 99.5% and the yield can be higher than 90%, so that the preparation method is a synthetic route very suitable for industrial production.

Description

Technical field: [0001] The invention relates to a preparation method of bupropion intermediate m-chloropropiophenone, which belongs to the field of medicine. Background of the invention: [0002] Bupropion is a new type of antidepressant developed by Glaxo Wellcome and launched in the United States in 1997. The product has an aminoketone structure and is a racemic mixture: [0003] [0004] This product was originally used clinically as an antidepressant, but during its use it was found that it can play a role in smoking cessation by blocking the reuptake of dopamine, serotonin and norepinephrine by nerves, so this product can also be used for Help smokers quit smoking. [0005] M-chloropropiophenone is the main intermediate for the synthesis of bupropion. It is a white crystalline powder with a melting point of 43-47°C and is easily soluble in most organic solvents: [0006] [0007] At present, the preparation method of the m-chloropropiophenone of bibliographica...

Claims

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Application Information

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IPC IPC(8): C07C49/807C07C45/63
CPCY02A50/20
Inventor 吴艳华吴荣贵陈钊李大军徐可岭
Owner WEIHAI DISU PHARMA CO LTD
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