Novel process for synthesizing 4-hydroxy-6-chloroquinoline

Abstract

The invention belongs to the technical field of synthesis of 4-hydroxy-6-chloroquinoline, and particularly relates to a novel process for synthesizing 4-hydroxy-6-chloroquinoline. The process comprises the following steps: S1, cleaning a first reaction container, drying and cooling the container to room temperature, adding parachloroaniline and 5-(methoxymethylene)-2, 2-dimethyl-1, 3-dioxo-4, 6-diketone into an ethanol solution with a certain concentration according to a molar ratio of (0.1-1):(0.1-1), performing slow stirring, and performing reacting for 4-6 hours until the reaction is finished; S2, carrying out suction filtration on the reaction product to obtain 80-95% A; S3, adding a certain amount of diphenyl ether-biphenyl eutectic into a second reaction container, heating the container to 240-260 DEG C, adding the product A, performing stirring,performing reacting for 5-10 minutes, and performing cooling to room temperature; and S4, carrying out suction filtration on a product obtained in the S3 in petroleum ether to obtain 80-90% 4-hydroxy-6-chloroquinoline, and performing drying to obtain a 4-hydroxy-6-chloroquinoline product. According to the method disclosed by the invention, spin-drying is changed into suction filtration, so that a solid product with very high purity can be obtained, and the time is also saved; and in addition, the diphenyl ether-biphenyl eutectic is used as the solvent, so that time, manpower and material resources can be saved.

Description

technical field [0001] The invention belongs to the technical field of 4-hydroxy-6 chloroquinoline synthesis and relates to a new synthesis process of 4-hydroxy-6 chloroquinoline. Background technique [0002] The defect of present 4-hydroxyl-6 chloroquinoline synthetic technique: [0003] 1. At present, ethanol is used as a solvent, and the reaction solution is directly spin-dried. There will be many small impurities in it, resulting in low purity of the product and a long reaction time. [0004] 2. Diphenyl ether eutectic is generally used as solvent, its melting point is about 26~30°C, and it is solid at room temperature. Diphenyl ether is used as solvent, which needs to be melted before use, which will increase the operating time, especially for a large number of reactions. A lot of time and manpower will be wasted. Contents of the invention [0005] The invention provides a new process for synthesizing 4-hydroxy-6-chloroquinoline, which can solve the problems pointe...

AI Technical Summary

Problems solved by technology

[0003] 1. At present, ethanol is used as a solvent, and the reaction solution is directly spin-dried. There will be many small impurities in it, resulting in low purity of the product and a long reaction time

[0004] 2. Diphenyl ether eutectic is generally used as solvent, its melting point is about 26~30°C, and it is solid at room temperature. Using diphenyl ether as solvent needs to be melted before use, which will increase the operating time, especially for a large number of reactions. It will waste a lot of time and manpower

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