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Preparation technology of carboxybenzaldehyde

A technology for the preparation of o-carboxybenzaldehyde, which is applied in the preparation of carboxylate salts, the preparation of organic compounds, organic chemistry, etc., can solve the problems of low yield of o-carboxybenzaldehyde, cumbersome preparation process steps, and poor controllability. Achieve the effects of convenient operation, simple preparation process steps and sufficient reaction

Inactive Publication Date: 2015-03-25
TAICANG YUNTONG BIOCHEM ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process steps are loaded down with trivial details, controllability is poor, and the o-carboxybenzaldehyde yield of preparation is low, and purity is low

Method used

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  • Preparation technology of carboxybenzaldehyde

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Embodiment 1

[0018] Embodiment 1: the preparation technology of a kind of o-carboxybenzaldehyde of the present embodiment comprises the following steps:

[0019] In terms of parts by mass, add 60 parts of chloroform and 120 parts of phthalide into the reaction kettle, heat to 105°C, pressurize to 8Mpa, add 100 parts of bromine water with a concentration of 80% dropwise within 1h and stir, and heat to 115 Reflux at 120°C for 1 hour, and pass nitrogen gas into the reactor for 1 hour at 120°C to make the reaction fully and remove hydrogen bromide gas, evaporate to dryness under reduced pressure to remove residual impurities, cool to 8°C, and dry at 20°C , to obtain 3-bromophthalide;

[0020] Add 40 parts of deionized water into the hydrolysis kettle, heat to 90°C, put in the 3-bromophthalide, heat in a water bath at 100°C for 2 hours, cool to 10°C, crystals are precipitated, and the wet product of o-carboxybenzaldehyde is obtained by suction filtration. Add o-carboxybenzaldehyde wet product ...

Embodiment 2

[0021] Embodiment 2: the preparation technology of a kind of o-carboxybenzaldehyde of the present embodiment comprises the following steps:

[0022] In terms of parts by mass, add 80 parts of chloroform and 120 parts of phthalide into the reaction kettle, heat to 105°C, pressurize to 8Mpa, add 110 parts of bromine water with a concentration of 80% dropwise within 1.2h, stir, and heat to Reflux at 115°C for 1 hour, and at 120°C, pass nitrogen gas into the reaction kettle for 1.2 hours to make the reaction fully and remove hydrogen bromide gas, evaporate to dryness under reduced pressure to remove residual impurities, cool to 8°C, and at 20°C Drying is carried out to obtain 3-bromophthalide;

[0023] Add 60 parts of deionized water into the hydrolysis kettle, heat to 90°C, put in the 3-bromophthalide, heat in a water bath at 100°C for 2 hours, cool to 10°C, precipitate crystals, and obtain the wet product of o-carboxybenzaldehyde by suction filtration. Add o-carboxybenzaldehyde...

Embodiment 3

[0024] Embodiment 3: the preparation technology of a kind of o-carboxybenzaldehyde of the present embodiment comprises the following steps:

[0025] In terms of parts by mass, add 100 parts of chloroform and 120 parts of phthalide into the reaction kettle, heat to 105°C, pressurize to 8Mpa, add 120 parts of bromine water with a concentration of 80% dropwise within 1.5h, stir, and heat to Reflux at 115°C for 1 hour, and at 120°C, pass nitrogen gas into the reaction kettle for 1.5 hours to make the reaction fully and remove hydrogen bromide gas, evaporate to dryness under reduced pressure to remove residual impurities, cool to 8°C, and in 20°C Drying is carried out to obtain 3-bromophthalide;

[0026] Add 80 parts of deionized water into the hydrolysis kettle, heat to 90°C, put in the 3-bromophthalide, heat in a water bath at 100°C for 2 hours, cool to 10°C, precipitate crystals, and obtain the wet product of o-carboxybenzaldehyde by suction filtration. Add o-carboxybenzaldehyd...

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Abstract

The invention discloses a preparation technology of carboxybenzaldehyde. The preparation technology comprises the following steps: (1) adding chloroform in a reaction kettle, adding phthalide, heating the chloroform and the phthalide, adding bromine water in a dripping manner, stirring the chloroform and the phthalide which are heated and the bromine, raising the temperature, and performing reflux; (2) adding nitrogen in the reaction kettle, performing decompressing and drying by distillation, performing cooling, precipitating crystals, performing suction filtration so as to obtain 3-bromine phthalide; (3) adding deionized water in a hydrolysis kettle, heating the deionized water for raising the temperature, adding the 3-bromine phthalide, performing water bath heating, performing cooling, precipitating crystals, performing suction filtration and obtaining a wet product of the carboxybenzaldehyde; (4) performing recrystallization on the wet product of the carboxybenzaldehyde and obtaining the carboxybenzaldehyde. The preparation technology disclosed by the invention has the advantages of simple steps and convenient operation, and the yield coefficient and the purity of the prepared carboxybenzaldehyde are high.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical intermediates, in particular to a preparation process of o-carboxybenzaldehyde. Background technique [0002] O-carboxybenzaldehyde is an important intermediate in the synthesis of antipyretic and analgesic drugs. Its CAS number is 119-67-52. It is a white to off-white crystalline powder with a melting point of 96-100°C. [0003] In the prior art, o-carboxybenzaldehyde is obtained by bromination and hydrolysis of phenol. Heat the phenol to react with bromine, and control the feed rate so that the reaction tail gas is basically discharged without bromine vapor. After cooling, o-carboxybenzaldehyde was precipitated. The preparation process has cumbersome steps and poor controllability, and the prepared o-carboxybenzaldehyde has low yield and low purity. Contents of the invention [0004] In view of this, the present invention provides a preparation process of o-carboxybenzaldehyde, which...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/30C07C51/373
CPCC07C51/373C07C65/30
Inventor 张卫东
Owner TAICANG YUNTONG BIOCHEM ENG
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