反应详情

457.2 g of 3-(2,4-dichlorophenyl)-5-difluoromethoxy-1H-pyrazole from Example 3.2 were initially charged in 2300 ml of toluene. 227.3 g of dimethyl sulfate were added dropwise, and the mixture was heated at reflux for 3 h. After cooling, 500 ml of saturated aqueous NH4Cl solution were added, the mixture was stirred for 1 h and the organic phase was separated off and washed with water until neutral. Drying over Na2SO4 and concentration gave 377.8 g of 3-(2,4-dichlorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole of a purity of 92.9% (GC). Yield: 73.1%. M.p.: 35° C.

1. temperaturethe mixture was heated
2. temperatureat reflux for 3 h
3. temperatureAfter cooling
4. customthe organic phase was separated off
5. washwashed with water until neutral
6. dry with materialDrying over Na2SO4 and concentration