反应详情

The compound from Step 5 (6.0 g, 9.7 mmol) was dissolved in 150 mL of ethanol and the solution was saturated with ammonia. The solution was let stand undisturbed overnight and then concentrated in vacuo. The residue was dissolved in ethyl acetate, washed with 1 N HCl and brine, dried over anhyd. MgSO4, filtered and concentrated in vacuo to afford N′-[[1-(4-(aminosulfonyl)phenyl]-5-(4-chlorophenyl)-1H-pyrazol-3-yl]methyl]-N′-hydroxyurea as a white solid that was crystallized from a mixture of ethyl acetate and hexane: mp 216-218° C.

1. customstand undisturbed overnight
2. concentrationconcentrated in vacuo
3. dissolutionThe residue was dissolved in ethyl acetate
4. washwashed with 1 N HCl and brine
5. customdried over anhyd
6. filtrationMgSO4, filtered
7. concentrationconcentrated in vacuo