反应详情

2.32 g (0.02 mol) of 1-(1,1-dimethyl-1-ethyl)-5-hydroxy-1H-pyrazole and 2.3 g (0.02 mol) of potassium carbonate were added to a solution of 5.4 g (0.02 mol) of 2-chloro-3-(4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoyl chloride in 100 ml of ethylene glycol dimethyl ether, and the mixture was stirred overnight. The mixture was subsequently refluxed for 3 hours, the solvent was distilled off, the residue was taken up in 300 ml of water and washed with methylene chloride and the aqueous phase was acidified to pH=3 using 10% strength hydrochloric acid. The precipitate was filtered off with suction and dried at 400° C. This gave 4.6 g (65% of theory) of 4-[2-chloro-3-(4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoyl]-5-hydroxy-1-(1,1-dimethyl-1-ethyl)-1H-pyrazole].

1. temperatureThe mixture was subsequently refluxed for 3 hours
2. distillationthe solvent was distilled off
3. washwashed with methylene chloride
4. filtrationThe precipitate was filtered off with suction
5. customdried at 400° C