Preparation method of difluorobenzodioxole

A technology of difluoropiperone and dichloropiperone, applied in the direction of organic chemistry and the like, can solve the problems of consuming hydrogen fluoride environment, high equipment requirements, complicated operation, etc., and achieves the effects of low equipment requirements, high yield, and mild reaction conditions

Pending Publication Date: 2022-03-15
山东福尔有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regardless of its authenticity, this patent by Sun Fuqiang et al. has the problems of rectification and removal of phosphorus oxychloride and phosphorus trichloride, high equipment requirements, and complicated operation. Dropping hydrogen fluoride under vacuum conditions will consume a large amount of hydrogen fluoride and cause environmental pollution. Pollution

Method used

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  • Preparation method of difluorobenzodioxole
  • Preparation method of difluorobenzodioxole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Check the 5000L chlorination kettle and its ancillary equipment to confirm that it is dry and clean, and the valve is closed. (There should be no accumulation of liquid in the kettle, phosphorus trichloride will release a lot of heat when it encounters water, and it may spray material). Open the vacuum valve of the chlorination kettle to evacuate to -0.08MPa, open the nitrogen valve and fill with nitrogen to replace the air in the chlorination kettle and the pipeline of the ancillary facilities, and replace it until the system pressure is normal pressure, and repeat this twice. Open the chlorination kettle vent valve, open the phosphorus trichloride feeding valve, and use a diaphragm pump to add 4332Kg of phosphorus trichloride into the reaction kettle chlorination kettle. Turn on the cooling oil of the jacket of the chlorination kettle in advance, the temperature of the kettle has dropped to 10-15°C, and the control temperature is less than 40°C, and 760Kg of chlorine ...

Embodiment 2

[0043] Check the 5000L chlorination kettle and its ancillary equipment to confirm that it is dry and clean, and the valve is closed. (There should be no accumulation of liquid in the kettle, phosphorus trichloride will release a lot of heat when it encounters water, and it may spray material). Open the vacuum valve of the chlorination kettle to evacuate to -0.08MPa, open the nitrogen valve and fill with nitrogen to replace the air in the chlorination kettle and the pipeline of the ancillary facilities, and replace it until the system pressure is normal pressure, and repeat this twice. Open the chlorination kettle vent valve, open the phosphorus trichloride feeding valve, and use a diaphragm pump to add 4332Kg of phosphorus trichloride into the reaction kettle chlorination kettle. Turn on the cooling oil of the jacket of the chlorination kettle in advance, the temperature of the kettle has dropped to 10-15°C, and the control temperature is less than 40°C, and 760Kg of chlorine ...

Embodiment 3

[0045] Check the 5000L chlorination kettle and its ancillary equipment to confirm that it is dry and clean, and the valve is closed. (There should be no accumulation of liquid in the kettle, phosphorus trichloride will release a lot of heat when it encounters water, and it may spray material). Open the vacuum valve of the chlorination kettle to evacuate to -0.08MPa, open the nitrogen valve and fill with nitrogen to replace the air in the chlorination kettle and the pipeline of the ancillary facilities, and replace it until the system pressure is normal pressure, and repeat this twice. Open the chlorination kettle vent valve, open the phosphorus trichloride feeding valve, and use a diaphragm pump to add 4332Kg of phosphorus trichloride into the reaction kettle chlorination kettle. Open the chlorination kettle jacket cooling oil in advance, the kettle temperature has dropped to 10-15℃, the control temperature is less than 60-70℃, 760Kg of chlorine gas is introduced, and the maxi...

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Abstract

The invention relates to a preparation method of difluorobenzodioxole, which comprises the following steps: step 1, introducing chlorine and phosphorus trichloride at 0-80 DEG C according to a molar ratio of 1: (3-9) to react to prepare phosphorus pentachloride, and after the phosphorus pentachloride is prepared, refluxing for 1-4 hours to enable the chlorine and the phosphorus trichloride to react completely so as to prevent the phosphorus pentachloride from adhering to the wall; 2, benzodioxole is dropwise added into phosphorus pentachloride for 1-24 h, and the molar ratio of benzodioxole to phosphorus pentachloride in phosphorus pentachloride is 1: (0.5-1.5); after dropwise adding, refluxing for 1-24 hours at the temperature of 50-100 DEG C; removing the phosphorus trichloride solvent to obtain dichlorobenzodioxole; and 3, reacting dichlorobenzodioxole with hydrogen fluoride according to the molar ratio of (1.8-8): 1, dropwise adding hydrogen fluoride into dichlorobenzodioxole for 0.5-24 hours, reacting at the reaction temperature of 5-40 DEG C for 0.5-24 hours after dropwise adding, adjusting the pH value to 7-14, and distilling with water vapor to obtain dichlorobenzodioxole. The method is simple and easy to implement, the difluorobenzodioxole is obtained with high yield and high purity, the cost is low, the reaction conditions are mild, and the method is suitable for industrial mass production.

Description

technical field [0001] The invention belongs to the field of preparation of difluoropiperonyl, in particular to a preparation method of difluoropiperonyl. Background technique [0002] Fludioxonil is a new type of contact protection bactericide with a unique mechanism of action. It inhibits the growth of pathogenic bacteria mycelium by inhibiting the transfer related to phosphorylation of glucose, and finally leads to the death of the bacteria. [0003] Difluoropiperone ring (full name: 2,2-difluoro-1,3-benzodioxin) is a colorless liquid with a boiling point of 129°C [0004] -130℃, it is a key intermediate in the synthesis of fludioxonil for agricultural fungicides. Yan Xiaomin et al ("World Pesticide", 2010, 32(3), 36-38) introduced the synthetic method of fludioxonil. [0005] The object of the present invention is to provide a kind of new preparation method of difluoropiperonyl, the method can easily, high yield, high purity obtain difluoropiperone ring, low cost, mild...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/46
CPCC07D317/46
Inventor 赵树清于天涌张名林范胜用杨海舰李鼎盛吴浩
Owner 山东福尔有限公司
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