反应详情

温度

50 °C

To a suspension of compound 3-2 (60 mg, 0.135 mmol) in H2O (100 mL) was added KOH (75 mg, 1.35 mmol) and stirred at 50° C. for 30 min. The reaction mixture was extracted with EA (20 mL). The aqueous layer was adjusted to pH 3 by addition of HCl. The solids were filtered to afford compound 3-3 as a white solid (40 mg, 71%). 1H NMR (300 MHz, DMSO-d6) δ 13.61 (br s, 1H), 10.02 (s, 1H), 8.99 (s, 1H), 7.35-7.26 (m, 12H), 5.76 (s, 1H). LC-MS: (M+H)+ 417.

1. extractionThe reaction mixture was extracted with EA (20 mL)
2. additionThe aqueous layer was adjusted to pH 3 by addition of HCl
3. filtrationThe solids were filtered