反应详情

The 2-amino-N-[[4-(5-methyl-3-phenylisoxazol-4-yl)phenyl]sulfonyl]acetamide (Example 81)(4.08 g, 10.9 mmol) was mixed in acetonitrile at room temperature. Triethylamine (3.03 g, 30.0 mmol) and acetic anhydride (1.23 g, 12.1 mmol) were added and the heterogeneous solution was stirred for 2 hours. The solution was vacuum filtered through a pad of diatomaceous earth and solvent was removed at reduced pressure. Water was added and the solution was stirred for 30 minutes. White crystals formed, were collected by vacuum filtration and dried to afford the desired product as a white solid (3.25 g, 78%): mp 218.2-219.3° C. 1H NMR (CD3OD/300 MHz) 8.01 (d, 2H, J=8.2 Hz), 7.42-7.36 (m, 7H), 3.85 (s, 2H), 2.50 (s, 3H), 1.95 (s, 3H). FABLRMS m/z 414 (M+H). Anal. Calc'd for C20H19N3O5S: C, 58.10; H, 4.63; N,10.16. Found: C, 58.18; H, 4.66; N, 10.14.

1. filtrationfiltered through a pad of diatomaceous earth and solvent
2. customwas removed at reduced pressure
3. additionWater was added
4. stirringthe solution was stirred for 30 minutes
5. customWhite crystals formed
6. filtrationwere collected by vacuum filtration
7. customdried