反应详情

温度

70 °C

A solution of Example 96C (0.073 g, 0.21 mmol) in methanol (4 mL) was treated with 2 mL conc. NaOH and heated to 70° C. for 18 hours. The mixture was concentrated, diluted with water, acidified to pH 5 with 1M HCl, and extracted with dichloromethane. The extract was dried (MgSO4), filtered, and concentrated to provide the desired product (0.010 g). MS (ESI(+)) m/e 329 (M+H)+; (ESI(−)) m/e 327 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 10.01 (dd, 1H), 8.97 (m, 1H), 8.30 (d, 1H), 7.92 (d, 1H), 7.74 (m, 5H), 7.54 (m, 1H).

1. concentrationThe mixture was concentrated
2. additiondiluted with water
3. extractionextracted with dichloromethane
4. dry with materialThe extract was dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated