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Preparation method for 3-hydroxyquinaldine-4-carboxylic acid

A technology of hydroxyquinaldine and carboxylic acid, which is applied in the field of preparing 3-hydroxyquinaldine-4-carboxylic acid, can solve the problems of high production cost and high usage of monochloroacetone, so as to improve efficiency, reduce usage, and reduce production cost effect

Inactive Publication Date: 2019-01-01
NANJING JINHAO MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Reference document CN 102070523 A discloses a new method for preparing 3-hydroxyquinaldine-4-carboxylic acid, in which the molar ratio of isatin, inorganic base and part of monochloroacetone is 1:1:1~ 2.0, the consumption of monochloroacetone is relatively high, and the production cost is high

Method used

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Embodiment

[0016] A kind of quinaldine---the preparation method of 3-hydroxyquinaldine-4-carboxylic acid, it comprises the steps:

[0017] (a), Synthesis of Oxime-Acetanilide: Add 300-800g of water, 250-500g of anhydrous sulfate and 40-100g of chloral in the flask, add 5-20g of inorganic acid after stirring and dissolving, and heat up to 35-55 ℃, add 36g of aniline and 55g of hydroxylamine in batches, raise the temperature to 78-88℃, keep it warm for 1-3h, rapidly cool to 30℃, continue stirring for 1h, filter, wash with water, and dry to obtain the product oximoacetanilide.

[0018] (b), using the oximoacetanilide obtained in step (a) to synthesize isatin: mix 300 g of concentrated sulfuric acid with 20 g of water, control the temperature below 30° C., add oxime acetanilide in batches, and control the temperature at 40 to 50° C. , the feeding time is 0.5-1h, and the reaction is kept in a 40°C water bath for 4-5h, and the material is slowly poured into a flask with 410g of water. , washe...

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Abstract

The invention discloses a preparation method for 3-hydroxyquinaldine-4-carboxylic acid. The preparation method comprises the following steps: 1) compounding oximide-acetanilide; 2) compounding isatinfrom oximide-acetanilide acquired in the step 1); 3) compounding quinaldine from the isatin acquired in the step 2): mixing 25-28g of calcium hydroxide, 20-28g of the isatin and 640-660g of water, dropwise adding 15-17g of monochloroacetone, rising temperature to 80-90 DEG C, reacting for 4-5h while preserving heat, and then cooling to 50 DEG C, dropwise adding a defined amount of hydrochloric acid, reacting for 0.5-1.5h while preserving heat, filtering, dissolving a filter cake in water, and meanwhile, adding ammonium chloride, rising temperature to 55 DEG C, preserving heat for 0.5-1h, filtering, washing with water, and drying, thereby obtaining a yellow product quinaldine. According to the invention, the ratio of the isatin to calcium hydroxide is adjusted, the actual usage amount of calcium hydroxide is reduced and the usage amount of monochloroacetone is consequently reduced, so that the production cost is lowered and the benefit is improved.

Description

technical field [0001] The present invention relates to a new method for preparing 3-hydroxyquinaldine-4-carboxylic acid. Background technique [0002] 3-Hydroxyquinaldine-4-carboxylic acid is the main intermediate for the preparation of C.I. Disperse Yellow 54 and 64. It is also a pharmaceutical intermediate. In conventional production technology, the process of synthesizing 3-hydroxyquinaldine-4-carboxylic acid with isatin as raw material is very mature. Reference document CN 102070523 A discloses a new method for preparing 3-hydroxyquinaldine-4-carboxylic acid, in which the molar ratio of isatin, inorganic base and part of monochloroacetone is 1:1:1~ 2.0, the consumption of monochloroacetone is higher, and the production cost is high. Contents of the invention [0003] The technical problem to be solved in the present invention is the relatively high defect of the use amount of monochloroacetone in the preparation technology of 3-hydroxyquinaldine-4-carboxylic acid, ...

Claims

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Application Information

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IPC IPC(8): C07D215/50
CPCC07D215/50
Inventor 吴建中刘伟强蒋利华王步成
Owner NANJING JINHAO MEDICAL TECH CO LTD