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Synthetic method for 3-aminoacetophenone

A technology of aminoacetophenone and a synthesis method, which is applied in the field of pharmaceutical intermediate synthesis, can solve the problems of polluted environment, high operation and maintenance cost, difficult purification and the like, and achieves the effects of high yield, low operation and maintenance cost, and simple technological process.

Inactive Publication Date: 2015-11-04
WUHAN RUIKAIXING SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, 3-aminoacetophenone is obtained by reducing 3-nitroacetophenone with iron powder, but the iron powder reduction method pollutes the environment, the equipment is severely corroded, the operation and maintenance costs are high, and continuous production is difficult.
Technologists have tried to prepare 3-aminoacetophenone by catalytic hydrogenation of 3-nitroacetophenone, but experiments have found that it is difficult to avoid the side effect that the ketone group on the 3-nitroacetophenone structure is reduced during the catalytic hydrogenation process. The occurrence of the reaction causes the purity of the target product to be low, the purification is difficult, and the yield is not high

Method used

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  • Synthetic method for 3-aminoacetophenone

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Effect test

Embodiment 1

[0025] A kind of synthetic method of 3-aminoacetophenone, its step is as follows:

[0026] (1) Preparation of additives: Disperse and dissolve 20 g of cobalt nitrate into 100 ml of ethanol, then add 5 g of magnesium oxide nanopowder, stir and sonicate at 40 Hz for 30 minutes, evaporate the ethanol solvent to dryness, and vacuum dry at 100 ° C After 10 hours, it is finally ground into a fine powder with a particle size of 0.5-2 microns to obtain an auxiliary agent.

[0027] (2) Add 40g of 3-nitroacetophenone, 160g of methanol, 3.5g of 1% palladium carbon catalyst and 2g of the auxiliary agent prepared in step (1) to the autoclave successively, at 60-70°C, pressure 0.5-0.6 Hydrogenation reaction under MPa, heat preservation reaction for 45 minutes, cooling to room temperature, filtration, and precipitation of the filtrate to obtain 3-aminoacetophenone with a yield of 97%.

Embodiment 2

[0029] A kind of synthetic method of 3-aminoacetophenone, its step is as follows:

[0030] (1) Preparation of additives: Disperse and dissolve 20g of nickel nitrate in 100ml of ethanol, then add 5g of magnesium oxide nanopowder, stir and sonicate at 40 Hz for 30 minutes, evaporate the ethanol solvent to dryness, and vacuum dry at 100°C After 10 hours, it is finally ground into a fine powder with a particle size of 0.5-2 microns to obtain an auxiliary agent.

[0031] (2) Add 40g of 3-nitroacetophenone, 160g of methanol, 3.5g of 1% palladium carbon catalyst and 2g of the auxiliary agent prepared in step (1) in the autoclave, at 60-70°C, pressure 0.5-0.6 Hydrogenation reaction under MPa, heat preservation reaction for 45 minutes, cooling to room temperature, filtration, and precipitation of the filtrate to obtain 3-aminoacetophenone with a yield of 95%.

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Abstract

The invention provides a synthetic method for 3-aminoacetophenone. The method comprises the following steps: (1) additive preparation: a step of dispersing and dissolving nitrate in an organic solvent, then adding oxide or carbonate nanometer powder, carrying out ultrasonic stirring, drying the organic solvent by distillation, carrying out vacuum drying, grinding the dried mixture into fine powder so as to obtain an additive; (2) successively adding 3-nitroacetophenone, methanol, a catalyst and the additive into a high-pressure kettle, carrying out hydrogenation reaction at certain temperature and pressure, then carrying out heat-preserving reaction time for certain time, carrying out cooling to room temperature, carrying out filtering, desolventizing obtained filtrate so as to obtain the 3-aminoacetophenone. The method provided by the invention has the advantages of high conversion rate, simple and convenient operation, high yield, low cost, easy industrialization production, safety and environmental protection.

Description

technical field [0001] The invention belongs to the technical field of synthesis of pharmaceutical intermediates, and in particular relates to a synthesis method of 3-aminoacetophenone. Background technique [0002] 3-Aminoacetophenone is used in the synthesis of phenylephrine drugs, the hypnotic drug zaleplon, etc., and can also be used as a raw material for organic synthesis. It is an important pharmaceutical intermediate and fine chemical, and is in demand in domestic and foreign markets. [0003] At present, 3-aminoacetophenone is obtained by reducing 3-nitroacetophenone with iron powder, but the iron powder reduction method pollutes the environment, the equipment is seriously corroded, the operation and maintenance costs are high, and continuous production is difficult. Technologists have tried to prepare 3-aminoacetophenone by catalytic hydrogenation of 3-nitroacetophenone, but experiments have found that it is difficult to avoid the side effect that the ketone group o...

Claims

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Application Information

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IPC IPC(8): C07C221/00C07C225/22B01J27/25
Inventor 游海军刘昱宁凡陈胜郑卓于巧璐牛小斌李诚
Owner WUHAN RUIKAIXING SCI & TECH
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