反应详情

温度

60 °C

A solution of Example 463A (1.37 g, 3.36 mmol) in methanol (31 mL) and distilled water (3.5 mL) was treated with lithium hydroxide monohydrate (0.704 g, 16.78 mmol), heated to 60° C. for 30 minutes, cooled to room temperature, treated with 1N HCl, and concentrated. The aqueous layer was extracted with dichloromethane twice and the combined organic fractions were dried (MgSO4), filtered, and concentrated to provide the desired product. MS (ESI(+)) m/e 396 (M+H)+; (ESI(−)) m/e 394 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 8.98 (br s, 1H), 7.89 (d, 1H), 7.33 (d, 1H), 7.12 (s, 2H), 3.77 (s, 3H), 2.67 (br s, 2H), 2.53 (br s, 2H), 1.65 (quint, 4H).

1. temperaturecooled to room temperature
2. concentrationconcentrated
3. extractionThe aqueous layer was extracted with dichloromethane twice
4. dry with materialthe combined organic fractions were dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated