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Method for producing bactericide prochloraz

A technology of prochloraz and fungicides, applied in the direction of fungicides, biocides, chemicals for biological control, etc., can solve the problem of large amount of wastewater

Active Publication Date: 2009-04-08
江苏乐斯化学有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to propose an improved prochloraz production method in view of the large amount of waste water in the current production process, which eliminates the washing operation except for the absorption of acid chloride waste gas and the recovery of triethylamine.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] In a 3000L etherification kettle, put 500kg of 99% 2,4,6-trichlorophenol, 750kg of dichloroethane, and 350kg of 30% liquid caustic soda, start stirring, seal and heat. The temperature is controlled at 125-135°C, the pressure is 0.80-0.85MPa, and the reaction is carried out for 10 hours. Cool down to 50-60°C, stop stirring, let stand for 1 hour, separate the lower water layer, and transfer the material to the still. Heat with stirring to distill out dichloroethane; when the temperature reaches above 100°C and there is no condensate in the condenser, change to vacuum. Control vacuum at 0.095-0.099MPa, temperature at 180-210°C, distill until there is no condensate in the condenser. Then 602 kg of 2,4,6-trichlorophenoxyethyl chloride was obtained, the content detected by HPLC was 99.47%, and the yield was 91.89% based on 2,4,6-trichlorophenol.

[0013] In a 3000L amination kettle, throw 602kg of 99.47% 2,4,6-trichlorophenoxyethyl chloride and 900kg of propylamine, and hea...

Embodiment 2

[0017] In a 3000L etherification kettle, put 500kg of 99% 2,4,6-trichlorophenol, 700kg of dichloroethane, and 350kg of 30% liquid caustic soda, start stirring, seal and heat. The temperature is controlled at 130-135°C, the pressure is 0.65-0.80MPa, and the reaction is carried out for 10 hours. Cool down to 60°C, stop stirring, and let stand for 1 hour. After the lower water layer is separated, the material is transferred to a still. Heat with stirring to distill out dichloroethane; when the temperature reaches above 100°C and there is no condensate in the condenser, change to vacuum. Control the vacuum at 0.095-0.098MPa, and the temperature at 180-210°C. When the vacuum is at 0.098MPa and there is no condensate in the condenser at a temperature of 220°C, stop heating and release the vacuum. Then 605 kg of 2,4,6-trichlorophenoxyethyl chloride was obtained, the content detected by HPLC was 99.6%, and the yield was 92.48% based on 2,4,6-trichlorophenol.

[0018] In a 3000L ami...

Embodiment 3

[0022]In a 3000L etherification kettle, put 500kg of 99% 2,4,6-trichlorophenol, 700kg of dichloroethane, and 350kg of 30% liquid caustic soda, start stirring, seal and heat. The temperature is controlled at 130-135°C, the pressure is 0.70-0.80 MPa, and the reaction is carried out for 9 hours. Cool down to 50°C, stop stirring, and let stand for 1 hour. After the lower water layer is separated, the material is transferred to a still. Heat and distill out dichloroethane while stirring; when the temperature reaches above 100°C and there is no condensate in the condenser, change to vacuuming. Control the vacuum at 0.095-0.098 MPa and the temperature at 180-210°C to evaporate 2,4,6-trichlorophenoxyethyl chloride. When the vacuum is at 0.098MPa and there is no condensate in the condenser at a temperature of 240°C, stop heating and release the vacuum. Then 618kg of 2,4,6-trichlorophenoxyethyl chloride was obtained, the content detected by HPLC was 98.58%, and the yield was 92.94% ba...

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PUM

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Abstract

The invention relates to a method for industrially producing disinfecting agent prochloraz, which is characterized by comprising the following steps: 2, 4, 6-trichlorophenol and dichloroethane taken as major raw materials directly react with propylamine after the 2, 4, 6- trichlorophenol and the dichloroethane are subjected to pressure condensation, are subjected to acyl chlorination through trichloromethyl carbonate, and react with imidazole to produce the prochloraz in the presence of triethylamine. Compared with the prior producing process, the method cancels intermediate washing, greatly reduces factory effluent, and improves product yield.

Description

Technical field: [0001] The invention relates to a production method of prochloraz, a pesticide fungicide, which is suitable for the production of prochloraz original drug by using 2,4,6-trichlorophenol and dichloroethane as main raw materials, and belongs to the field of pesticide chemical industry. Background technique: [0002] Prochloraz (Prochloraz), the chemical name is N-propyl-N-(2,4,6-trichlorophenoxyethyl)-1H-imidazole-1-carboxamide, is a British Boots Co., Ltd. in Synthesized in 1974 and introduced to the market in 1977, it is an imidazole-based high-density broad-spectrum fungicide. It works by inhibiting the biosynthesis of sterols, and has a good control effect on various pathogens of rice, fruits, and cereals. [0003] There are many preparation methods of prochloraz, and the process route is complicated. In 1976, US Patent No. 3 991 071 described a preparation method using 2,4,6-trichlorophenol and dibromoethane as main raw materials. Dibromoethane is known...

Claims

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Application Information

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IPC IPC(8): C07D233/58A01P3/00
Inventor 张捷龙陈呈新雷进海
Owner 江苏乐斯化学有限公司
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