反应详情

To a solution of crude 2-(1-{[4-iodo-2-(trifluoromethyl)phenyl]methyl}-1H-pyrazol-3-yl)-1H-isoindole-1,3(2H)-dione (1.7 g, 3.42 mmol) in THF (30 ml) was added hydrazine monohydrate (0.83 ml, 17.1 mmol, Aldrich). The resulting yellow solution was stirred at ambient temperature under nitrogen for 5 h. The resulting suspension was filtered using a hydrophobic frit and the residue washed with ether (approximately 25 ml). The filterate was concentrated in vacuo and the residue loaded in dichloromethane and purified on silica 100 g using 0-100% ethyl acetate-dichloromethane+0-20% methanol (+1% Et3N). The appropriate fractions were combined and evaporated in vacuo to give the title compound as a pale yellow solid (0.624 g); LCMS: (System 4) MH+=368, tRET=2.54 min.

1. filtrationThe resulting suspension was filtered
2. washthe residue washed with ether (approximately 25 ml)
3. concentrationThe filterate was concentrated in vacuo
4. custompurified on silica 100 g
5. customevaporated in vacuo