反应详情

温度

55 °C

To a 200 mL round bottomed flask was added 7 (1 g, 4.5 mmol) suspended in 1 N NaOH (35 mL). The reaction mixture was heated at 55° C. for 3 h. The resulting solution was cooled in an ice bath and neutralized with AcOH. The precipitated solid was collected by filtration, washed with brine, and dried in vacuo to afford 0.67 g (92%) of 8 as a white solid: mp 252-254° C.; TLC Rf0.15 (MeOH/CHCl3, 1:5); 1H NMR (DMSO-d6) δ 2.20 (s, 3 H), 5.65 (s, 1 H), 5.65 (s, 2 H), 10.21 (s, 1 H), 11.15 (s, 1 H). Anal. (C7H8N4O0.73H2O) C, H, N.

1. temperatureThe resulting solution was cooled in an ice bath
2. filtrationThe precipitated solid was collected by filtration
3. washwashed with brine
4. customdried in vacuo