反应详情

温度

75 °C

A mixture of 4-chloro-8-(cyclopentyloxy)-7-methoxy-2H-chromen-2-one (170 mg, 0.58 mmol, Example 7, Step 1), glycinamide•HCl (77 mg, 0.70 mmol), triethylamine (0.2 mL, 1.4 mmol), and ethanol (2 mL) was heated at 75° C. in a sealed vial for 30 h. The reaction was allowed to cool to rt, concentrated, diluted with dichloromethane (10 mL), and let stand. After 10 min, the free-flowing solid was filtered and dried to give 2-(8-(cyclopentyloxy)-7-methoxy-2-oxo-2H-chromen-4-ylamino)acetamide: 1H NMR (400 MHz, DMSO-d6): δ 7.89 (t, 1H), 7.70 (d, 1H), 7.57 (s, 1H), 7.22 (s, 1H), 7.07 (d, 1H), 4.83 (s, 1H), 4.81 (m, 1H), 3.86 (s, 3H), 3.80 (d, 2H), 1.90-1.48 (m, 8H); MS (ESI): 333.0.

1. temperatureto cool to rt
2. concentrationconcentrated
3. additiondiluted with dichloromethane (10 mL)
4. filtrationthe free-flowing solid was filtered
5. customdried