Green synthesis method of oxine-copper technical material

Abstract

The invention discloses a green synthesis method of oxine-copper technical material The preparation method comprises the following steps: reacting 8-hydroxyquinoline with copper salt in water under the catalysis of dilute sulfuric acid to obtain oxine-copper containing crystal water, wherein the copper salt is basic cupric carbonate or copper hydroxide. According to the invention, basic cupric carbonate or copper hydroxide is used as a copper source, a catalytic amount of sulfuric acid is used as a catalyst, water is used as a solvent, and a complexing reaction is carried out to obtain the oxine-copper technical material. The technological process of the synthesis method is more environmentally friendly, a reaction solvent is water, reaction byproducts are carbon dioxide and water, and a large amount of inorganic waste salt is not generated; the reaction process is mild, the reaction conversion rate is high, and the reaction process is fast; wherein the prepared product is a green quinoline copper raw drug containing crystal water.

Description

technical field

[0001] The invention relates to a green synthesis method of quinoline copper raw drug, which belongs to the technical field of organic synthesis. Background technique

[0002] Copper quinoline is a chemical substance, yellow to green powder, non-volatile, non-deliquescent, black at high temperature, insoluble in water and most solvents. Copper quinoline can be used as a pharmaceutical synthetic metal corrosion inhibitor; it is used as a fungicide in agriculture; it is also used as a fungicide for ropes, threads, leather, and vinyl plastics; it is used as a fungicide in agriculture to prevent and control bacterial horns in cucumbers Spot disease, mango bacterial angular spot, citrus canker, apple tree ring spot, etc.

[0003] The existing production method is to use 8-hydroxyquinoline and copper sulfate, copper chloride, copper acetate, etc. as raw materials for chelation reaction to obtain copper quinoline. After the reaction, hydrogen equivalent to 8-hydrox...

Examples

Embodiment 1

[0021] Embodiment 1, green efficient synthesis of quinoline copper original drug

[0022] At room temperature (25°C), add 100g of 8-hydroxyquinoline, 40g of basic copper carbonate and 280g of water to a reactor with a stirring condensing reflux device, and slowly add 50% sulfuric acid dropwise to the above system under stirring Solution 1g, in this embodiment, the mass ratio of 8-hydroxyquinoline, basic copper carbonate and dilute sulfuric acid is 200:80:1, heat up to 50°C, keep warm for 2 hours, then heat up to 75°C, keep warm for 1 After the reaction was completed, it was naturally cooled to room temperature.

[0023] Suction filter the reaction system after cooling and crystallization, and wash the obtained solid product with water three times, each time with about 150 g of water; transfer the obtained solid product to an oven, and dry it at 80°C for 12 hours to obtain the green copper quinoline original drug. Weighing 133.7g, the liquid chromatography detection content is...

Embodiment 2

[0028] Embodiment 2, the green high-efficiency synthesis of quinoline copper original drug

[0029] At room temperature (25°C), add 400g of 8-hydroxyquinoline, 135g of copper hydroxide, and 1500g of water to a reactor with a stirring condensing reflux device, and slowly add 30% sulfuric acid solution dropwise to the above system under stirring 6g, in this example, the mass ratio of 8-hydroxyquinoline, basic copper carbonate and dilute sulfuric acid is 222:75:1, the temperature is raised to 60°C, and the reaction is kept for 2 hours, then the temperature is raised to 80°C, and the reaction is kept for 1 hour . After the reaction was completed, it was naturally cooled to room temperature.

[0030] Suction filter the reaction system after cooling and crystallization, and wash the obtained solid product with water three times, with a water consumption of about 600g each time; transfer the obtained solid product to an oven, and dry it at 80°C for 12 hours to obtain the green coppe...

technical field

[0001] The invention relates to a green synthesis method of quinoline copper raw drug, which belongs to the technical field of organic synthesis. Background technique

[0002] Copper quinoline is a chemical substance, yellow to green powder, non-volatile, non-deliquescent, black at high temperature, insoluble in water and most solvents. Copper quinoline can be used as a pharmaceutical synthetic metal corrosion inhibitor; it is used as a fungicide in agriculture; it is also used as a fungicide for ropes, threads, leather, and vinyl plastics; it is used as a fungicide in agriculture to prevent and control bacterial horns in cucumbers Spot disease, mango bacterial angular spot, citrus canker, apple tree ring spot, etc.

[0003] The existing production method is to use 8-hydroxyquinoline and copper sulfate, copper chloride, copper acetate, etc. as raw materials for chelation reaction to obtain copper quinoline. After the reaction, hydrogen equivalent to 8-hydrox...

Examples

Embodiment 1

[0021] Embodiment 1, green efficient synthesis of quinoline copper original drug

[0022] At room temperature (25°C), add 100g of 8-hydroxyquinoline, 40g of basic copper carbonate and 280g of water to a reactor with a stirring condensing reflux device, and slowly add 50% sulfuric acid dropwise to the above system under stirring Solution 1g, in this embodiment, the mass ratio of 8-hydroxyquinoline, basic copper carbonate and dilute sulfuric acid is 200:80:1, heat up to 50°C, keep warm for 2 hours, then heat up to 75°C, keep warm for 1 After the reaction was completed, it was naturally cooled to room temperature.

[0023] Suction filter the reaction system after cooling and crystallization, and wash the obtained solid product with water three times, each time with about 150 g of water; transfer the obtained solid product to an oven, and dry it at 80°C for 12 hours to obtain the green copper quinoline original drug. Weighing 133.7g, the liquid chromatography detection content is...

Embodiment 2

[0028] Embodiment 2, the green high-efficiency synthesis of quinoline copper original drug

[0029] At room temperature (25°C), add 400g of 8-hydroxyquinoline, 135g of copper hydroxide, and 1500g of water to a reactor with a stirring condensing reflux device, and slowly add 30% sulfuric acid solution dropwise to the above system under stirring 6g, in this example, the mass ratio of 8-hydroxyquinoline, basic copper carbonate and dilute sulfuric acid is 222:75:1, the temperature is raised to 60°C, and the reaction is kept for 2 hours, then the temperature is raised to 80°C, and the reaction is kept for 1 hour . After the reaction was completed, it was naturally cooled to room temperature.

[0030] Suction filter the reaction system after cooling and crystallization, and wash the obtained solid product with water three times, with a water consumption of about 600g each time; transfer the obtained solid product to an oven, and dry it at 80°C for 12 hours to obtain the green coppe...