A kind of synthetic method of fuconazole

Abstract

The invention relates to a method for synthesizing triazolol, which comprises reacting methyl halide and dimethyl sulfoxide at 0-120°C for 1-48 hours; adding solid base and 2,4'-difluorobenzophenone, the temperature Control at 0-80°C, react for 1-25h; add triazole, control the temperature at 50-200°C, react for 1-20h, after the reaction, filter, remove the solvent, wash, and crystallize to obtain the triazole . Dimethyl sulfoxide in the present invention is not only used as a reaction raw material, but also as a solvent, which avoids the difficulty of separation of mixed solvents, and dimethyl sulfoxide and methyl halide replace the dimethyl sulfoxide that has a large environmental pressure in the prior art. Sulfur ether and highly toxic chemical dimethyl sulfate, so that the present invention is environmentally friendly. In addition, the present invention has mild reaction conditions, short reaction time, high yield, high product quality, low discharge of three wastes, and only produces a single inorganic salt , thus the present invention has high production capacity and good economic efficiency.

Description

technical field

[0001] The invention belongs to the field of pesticide chemical industry, and in particular relates to a method for synthesizing triconazole. Background technique

[0002] Triazole, the abbreviation of 1-(2-fluorophenyl)-1-(4-fluorophenyl)-1-hydrogen-1,2,4-triazole-ethanol, is a protective and therapeutic Systemic triazole fungicides can be absorbed by roots, stems, and leaves, and can quickly conduct upwards in plants to prevent and control diseases caused by Ascomycetes, Basidiomycetes, and Deuteromycetes, especially for total erosion of wheat Disease, powdery mildew, rust, root rot, rice bad fungus, banana leaf spot have good control effect.

[0003] At present, the mainstream process of synthesizing futriazole is divided into two steps. One is to prepare sulfonium salt from dimethyl sulfide and dimethyl sulfate, add solid base and 2,4'-difluorobenzophenone, and remove After removing unreacted raw materials and reaction solvents, extracting, washing with...

Examples

Embodiment 1

[0040] Add 156g DMSO to the reactor, raise the temperature to 35-40°C, start to feed 50g of methyl chloride gas, the ventilation rate is not higher than 20g / h, the ventilation time is 2-3h, and keep warm at 35-40°C for 3h after the ventilation is completed. After the reaction, lower the temperature to 30-35°C and add 45g of sodium hydroxide in batches. After adding the sodium hydroxide, start to add 145g of 2,4'-difluorobenzophenone dropwise at a rate of 80g / h. The temperature is controlled at 30-40°C. After the dropwise addition, keep warm for 3 hours, then add 50 g of DMSO, add 55 g of triazole in batches, raise the temperature to 130-140° C., take samples for analysis after keeping warm for 2 hours, and the reaction is over. After the reaction, the temperature of the reactor was lowered to 50-60° C., the solid salt was filtered out by pressure filtration, and 30 g of DMSO was used to wash the solid salt. The filtered reaction solution was desolvated, and DMSO was recovered...

Embodiment 2

[0042] Add 156g DMSO to the reactor, raise the temperature to 35-40°C, start to feed 50g of methyl chloride gas, the ventilation rate is not higher than 20g / h, the ventilation time is 2-3h, and keep warm at 35-40°C for 3h after the ventilation is completed. After the reaction, lower the temperature to 30-35°C and add 45g of sodium hydroxide in batches. After adding the sodium hydroxide, start to add 145g of 2,4'-difluorobenzophenone dropwise at a rate of 80g / h. The temperature is controlled at 30-40°C. After the dropwise addition, keep warm for 3h, then add 250g of DMSO, add 55g of triazole in batches, raise the temperature to 130-140°C, keep warm for 2h, take samples for analysis, and the reaction is over. After the reaction, the temperature of the reactor was lowered to 50-60° C., the solid salt was filtered out by pressure filtration, and 30 g of DMSO was used to wash the solid salt. The filtered reaction solution was desolvated, and DMSO was recovered for reuse. Add 500g...

Embodiment 3

[0044]Add 156g DMSO to the reactor, raise the temperature to 35-40°C, start to feed 50g of methyl chloride gas, the ventilation rate is not higher than 20g / h, the ventilation time is 2-3h, and keep warm at 35-40°C for 3h after the ventilation is completed. After the reaction, lower the temperature to 30-35°C and add 35g of sodium hydroxide in batches. After adding the sodium hydroxide, start to add 145g of 2,4'-difluorobenzophenone dropwise at a rate of 80g / h. The temperature is controlled at 30-40°C. After the dropwise addition, keep warm for 3 hours, then add 10g of sodium hydroxide and 250g of DMSO, add 55g of triazole in batches, raise the temperature to 90-100°C, take samples for analysis after keeping warm for 7 hours, and the reaction is over. After the reaction, the temperature of the reactor was lowered to 50-60° C., the solid salt was filtered out by pressure filtration, and 30 g of DMSO was used to wash the solid salt. The filtered reaction solution was desolvated,...

technical field

[0001] The invention belongs to the field of pesticide chemical industry, and in particular relates to a method for synthesizing triconazole. Background technique

[0002] Triazole, the abbreviation of 1-(2-fluorophenyl)-1-(4-fluorophenyl)-1-hydrogen-1,2,4-triazole-ethanol, is a protective and therapeutic Systemic triazole fungicides can be absorbed by roots, stems, and leaves, and can quickly conduct upwards in plants to prevent and control diseases caused by Ascomycetes, Basidiomycetes, and Deuteromycetes, especially for total erosion of wheat Disease, powdery mildew, rust, root rot, rice bad fungus, banana leaf spot have good control effect.

[0003] At present, the mainstream process of synthesizing futriazole is divided into two steps. One is to prepare sulfonium salt from dimethyl sulfide and dimethyl sulfate, add solid base and 2,4'-difluorobenzophenone, and remove After removing unreacted raw materials and reaction solvents, extracting, washing with...

Examples

Embodiment 1

[0040] Add 156g DMSO to the reactor, raise the temperature to 35-40°C, start to feed 50g of methyl chloride gas, the ventilation rate is not higher than 20g / h, the ventilation time is 2-3h, and keep warm at 35-40°C for 3h after the ventilation is completed. After the reaction, lower the temperature to 30-35°C and add 45g of sodium hydroxide in batches. After adding the sodium hydroxide, start to add 145g of 2,4'-difluorobenzophenone dropwise at a rate of 80g / h. The temperature is controlled at 30-40°C. After the dropwise addition, keep warm for 3 hours, then add 50 g of DMSO, add 55 g of triazole in batches, raise the temperature to 130-140° C., take samples for analysis after keeping warm for 2 hours, and the reaction is over. After the reaction, the temperature of the reactor was lowered to 50-60° C., the solid salt was filtered out by pressure filtration, and 30 g of DMSO was used to wash the solid salt. The filtered reaction solution was desolvated, and DMSO was recovered...

Embodiment 2

[0042] Add 156g DMSO to the reactor, raise the temperature to 35-40°C, start to feed 50g of methyl chloride gas, the ventilation rate is not higher than 20g / h, the ventilation time is 2-3h, and keep warm at 35-40°C for 3h after the ventilation is completed. After the reaction, lower the temperature to 30-35°C and add 45g of sodium hydroxide in batches. After adding the sodium hydroxide, start to add 145g of 2,4'-difluorobenzophenone dropwise at a rate of 80g / h. The temperature is controlled at 30-40°C. After the dropwise addition, keep warm for 3h, then add 250g of DMSO, add 55g of triazole in batches, raise the temperature to 130-140°C, keep warm for 2h, take samples for analysis, and the reaction is over. After the reaction, the temperature of the reactor was lowered to 50-60° C., the solid salt was filtered out by pressure filtration, and 30 g of DMSO was used to wash the solid salt. The filtered reaction solution was desolvated, and DMSO was recovered for reuse. Add 500g...

Embodiment 3

[0044]Add 156g DMSO to the reactor, raise the temperature to 35-40°C, start to feed 50g of methyl chloride gas, the ventilation rate is not higher than 20g / h, the ventilation time is 2-3h, and keep warm at 35-40°C for 3h after the ventilation is completed. After the reaction, lower the temperature to 30-35°C and add 35g of sodium hydroxide in batches. After adding the sodium hydroxide, start to add 145g of 2,4'-difluorobenzophenone dropwise at a rate of 80g / h. The temperature is controlled at 30-40°C. After the dropwise addition, keep warm for 3 hours, then add 10g of sodium hydroxide and 250g of DMSO, add 55g of triazole in batches, raise the temperature to 90-100°C, take samples for analysis after keeping warm for 7 hours, and the reaction is over. After the reaction, the temperature of the reactor was lowered to 50-60° C., the solid salt was filtered out by pressure filtration, and 30 g of DMSO was used to wash the solid salt. The filtered reaction solution was desolvated,...

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