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Purification method of quinaldine

A purification method, quinaldine technology, applied in the field of high-purity quinaldine, can solve the problem of low purity of finished products, and achieve the effect of easy operation

Active Publication Date: 2009-09-16
XIANGSHUI HENRYDA TECH CHEM
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Problems solved by technology

[0007] The method is simple and easy to operate, but the calcium ion content in the quinaldine product is as high as 4800mg / kg, and the purity of the finished product is low (only about 90%)

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Embodiment Construction

[0018] Specific embodiments of the present invention will be described below, but not limited to this embodiment.

[0019] Add 400ml of water to a 1000ml four-neck flask, add 150g of calcium oxide, then add 14.7g (0.1mol) of isatin, raise the temperature to 65-80°C, add 12g of monochloroacetone dropwise, the temperature is 85-90°C, and react 5 A product solution containing quinaldine was obtained in 1 hour.

[0020] Cool the above product solution to 60°C, adjust the pH to 8-9 with 30% sodium hydroxide solution, filter, and keep the filtrate;

[0021] The resulting filtrate was adjusted to pH 4-5 with hydrochloric acid at 60-65°C, precipitated, filtered, washed with water, and the filter cake was dried to obtain 19 grams of finished quinaldine. After chemical analysis, the finished product has a purity of 95%, and the calcium ion content is about 450mg / kg.

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Abstract

The invention provides a purification method of quinaldine prepared by isatin, comprising: dissolving quinaldine in alkali solution in concentration of 10-40 mass% at 10-70 DEG C, or adding alkali solution in concentration of 10-40 mass% into the reaction product solution obtained from the quinaldine preparation by isatin; controlling the p H value of the quinaldine aqueous solution at 8-9, filtering and preserving filtrate; then adding acid into the above filtrate at 50-70 DEG C, adjusting p H of the filtrate at 4-5. filtering, clearing filter cake, drying to obtain quinaldine pure product. The calcium ion content in the purified quinaldine product is below 500mg / kg and the purify of the quinaldine is above 95%. In addition, the purification method is simple and easy to operate.

Description

technical field [0001] The invention relates to a method for purifying quinaldine prepared from isatin so as to obtain high-purity quinaldine. Background technique [0002] Quinaldine (3-hydroxyquinaldine-4-carboxylic acid) is the main intermediate for the preparation of C.I. Disperse Yellow 54 and 64, and it is also the main intermediate for the synthesis of high-grade acid dyes. In the prior art, one of the preparation methods of quinaldine is to synthesize isatin as a raw material, and the method mainly includes the following steps: [0003] 1. Substitution reaction: The hydroxyl substitution reaction between monochloroacetone and calcium hydroxide produces 1-hydroxyacetone. The equation expresses: [0004] [0005] 2. Condensation reaction: the product of step 1 undergoes a condensation reaction with isatin in an aqueous medium, and re-closes the ring to generate a quinaldine product. represented by the following reaction equation: [0006] [0007] The method i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/50
Inventor 张正富蒋利荣
Owner XIANGSHUI HENRYDA TECH CHEM
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