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Process of synthesizing alpha-(N-methyl-N-benzylamin)-3-hydroxy acetophenone hydrochloride

A technology of hydroxyacetophenone hydrochloride and synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as low product purity, achieve simplified process, simple and easy environmental management, The effect of improving the production environment

Inactive Publication Date: 2007-12-19
TAIZHOU MINGXIANG 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 benzoic acid that is hydrolyzed, 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-N-benzylamino)-3-hydroxyacetophenone hydrochloride with less waste and environmental friendliness

Method used

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  • Process of synthesizing alpha-(N-methyl-N-benzylamin)-3-hydroxy acetophenone hydrochloride
  • Process of synthesizing alpha-(N-methyl-N-benzylamin)-3-hydroxy acetophenone hydrochloride
  • Process of synthesizing alpha-(N-methyl-N-benzylamin)-3-hydroxy acetophenone hydrochloride

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Experimental program
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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. Use a low-vacuum four-stage low-cooled water absorption device to recover hydrogen bromide gas, dropwise, keep warm for 5 minutes, cool to 20°C, and discharge to a 1000L reaction pot (wherein there is 100kg of water at 0°C), and continue stirring after discharging 5 minutes, let stand for 30 minutes, separate the lower water layer, extract the water layer with 100kg hydrochloric acid recovered butyl acetate once...

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Abstract

The present invention is process of synthesizing alpha-(N-methyl-N-benzylamido)-3-hydroxy acetophenone hydrochloride. Alpha-(N-methyl-N-benzylamido)-3-hydroxy acetophenone hydrochloride is synthesized with 3-acetoxy acetophenone and methylbenzyl amine as main materials, and butyl acetate as solvent, and through bromizing, amination and hydrolysis reaction. The present invention has the features of simple technological process, facile materials, high product yield, high product purity, low cost, environment friendship, etc.

Description

technical field [0001] The invention relates to a synthesis method of α-(N-methyl-N-benzylamino)-3-hydroxyacetophenone hydrochloride. 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-N-benzylamino)-3-hydroxyacetophenone hydrochloride, referred to as BAH, is the key intermediate for the preparation of phenylephrine hydrochloride (ie, phenylephrine), with the following three route. [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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C221/00C07C225/14
Inventor 赵大同
Owner TAIZHOU MINGXIANG CHEM
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