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Process for synthesizing alpha-(N-methyl-benzyl)-3-hydroxy acetophenone

A technology of hydroxyacetophenone and its synthetic method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve the problem of low product purity

Active Publication Date: 2006-12-27
JIANGSU YUXIANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0017] The object of the invention aims at the toxic solvents such as chloroform and benzene that exist in the prior art, and the product contains hydrolyzed benzoic acid, which is difficult to completely remove from the product, and the problem that the product purity is not high provides a simple and convenient process, low cost, Synthetic method of α-(N-methyl-benzyl)-3-hydroxyacetophenone with less waste and environmental friendliness

Method used

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  • Process for synthesizing alpha-(N-methyl-benzyl)-3-hydroxy acetophenone
  • Process for synthesizing alpha-(N-methyl-benzyl)-3-hydroxy acetophenone
  • Process for synthesizing alpha-(N-methyl-benzyl)-3-hydroxy acetophenone

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Embodiment

[0040] Feeding amount of wet crude product (single pot)

[0041] Butyl acetate: 300kg (one barrel) Nitrogen: 3 bottles

[0042] 3-Acetoxyacetophenone: 178kg

[0043] Bromine: 160kg

[0044] Sodium carbonate: 58kg

[0045] N-Methylbenzylamine: 121kg Butyl acetate: 300kg

[0046] Hydrochloric acid: 100kg

[0047] Sodium chloride: 300kg

[0048] 1. Put 300kg of butyl acetate and 178kg of 3-acetoxyacetophenone into a 500L reaction pot, stir for 15 minutes, and add dropwise 160kg of bromine previously pumped into the high level tank at an internal temperature of 20°C. Reclaim hydrogen bromide gas with low vacuum four-stage low-cooled water absorption device, dropwise, keep warm for 5 minutes, cool to 20°C, discharge to 1000L reaction pot (wherein there is 100kg of water at 0°C), after discharging, continue to stir for 5 Minutes, let stand for 30 minutes, separate the lower water layer, extract the water layer with 100kg of hydrochloric acid and recover butyl acetate once, dis...

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Abstract

The invention relates to a method for synthesizing alpha-(N-methyl-benzyl)-3-hydroxy acetyl benzene, taking 3-acetoxy acetyl benzene and methyl-benzyl amine as main raw material, taking single butyl acetate as dissolvent and comprising bromation, amination and hydrolytic reaction. It is characterized by simple process, easy-getable raw material, no usage of inflammable, explosive and toxic chemical dissolvent, and increased productivity by 5%, high purity, low cost and little waste.

Description

technical field [0001] The invention relates to a synthesis method of α-(N-methyl-benzyl)-3-hydroxyacetophenone. Background technique [0002] Phenylephrine hydrochloride, also known as phenylephrine, is an adrenaline-mimetic drug that constricts local blood vessels. It is mainly used in surgical operations to prolong the time of local anesthesia. Pupil and symptoms of acute hypotension and abnormal heart beat, the products have a large demand in their respective fields. [0003] α-(N-methyl-benzyl)-3-hydroxyacetophenone, referred to as BAH, is a key intermediate for the preparation of phenylephrine hydrochloride (ie phenylephrine), and has the following three routes. [0004] [1] Sergievskaya, S.I.; Ravdel, G.A., Zhumal Obshchei Khimii (1952), 22 496-502., using 3-benzoyloxyacetophenone, methyl benzylamine, etc. as main raw materials, after bromination, Amination, hydrolysis and other reactions in the system. Its reaction formula is as follows: [0005] [0006] In t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C221/00C07C225/06
Inventor 赵大同
Owner JIANGSU YUXIANG CHEM
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