反应详情

A mixture 1-phenyl-3-trifluoromethyl-4-chloropyrazole (524 mg; 2 mmol), 2-bromomethyl-4-isopropyl-6-methoxy-1,2-benzisothiazol-3(2H)-one 1,1-dioxide (696 mg, 2 mmol), and KF (232 mg; 4 mmol) in DMF (8 ml) was stirred at 20° C. for 16 hours and the mixture was diluted with water. The above mixture was extracted with methylene chloride (3×) and the organic layer was dried over sodium sulfate, and concentrated in vacuo. The white residue was recrystallized from methylene chloride/hexane and purified by column chromatography (silica gel; 20% ethyl acetate/hexane; methylene chloride) to afford 730 mg (69%) of 4-isopropyl-6-methoxy-2-(1-phenyl-3-trifluoromethyl-4-chloropyrazol-5-yl-oxymethyl)-1,2-benzisothiazol-3(2H)-one 1,1-dioxide (Formula I: R1 =Ph; R2 =CF3 ; R3 =Cl; R4 =CH(CH3)2 ; R5 =6-OCH3) as a white solid, m.p. 185°-1870° C.

1. extractionThe above mixture was extracted with methylene chloride (3×)
2. dry with materialthe organic layer was dried over sodium sulfate
3. concentrationconcentrated in vacuo
4. customThe white residue was recrystallized from methylene chloride/hexane
5. custompurified by column chromatography (silica gel; 20% ethyl acetate/hexane; methylene chloride)