Novel process for synthesizing 4-hydroxy-6-chloroquinoline

A chloroquinoline and new process technology, which is applied in the field of 4-hydroxy-6 chloroquinoline synthesis new process, can solve the problems of long reaction time, waste of time and labor, low product purity, etc., and achieves the effect of saving labor and time

Inactive Publication Date: 2021-06-15
DEZHOU UNIV
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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 sol

Method used

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  • Novel process for synthesizing 4-hydroxy-6-chloroquinoline

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Embodiment Construction

[0016] A specific embodiment of the present invention will be described in detail below, but it should be understood that the protection scope of the present invention is not limited by the specific embodiment.

[0017] refer to figure 1 Shown, a kind of 4-hydroxyl-6 chloroquinoline synthetic new technique comprises the following steps:

[0018] S1. Clean the first reaction container, dry it, cool it to room temperature, and mix p-chloroaniline and 5-(methoxymethylene)-2,2-dimethyl-1,3-dioxo-4,6-diketone Put it into a certain concentration of ethanol solution at a molar ratio of 0.1-1:0.1-1, stir slowly, and react for 4-6 hours until the reaction is complete. The reaction conditions are normal temperature and pressure, and it is synthesized by a one-pot method;

[0019] S2, the reaction product is suction-filtered to obtain 80%-95% of A, and the method of suction filtration is simple, quick, green and environmentally friendly, and the obtained product has high purity;

[002...

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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...

Claims

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Application Information

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IPC IPC(8): C07D215/233
CPCC07D215/233
Inventor 华玉山姜云奎李荣春魏荣敏杨敏
Owner DEZHOU UNIV
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