反应详情

温度

50 °C

To a solution of Compound 46d (1.1 g, 3.2 mmol) in MeOH (20 mL) and THF (20 mL) was added 7 N NaOH (4.0 mL, 28 mmol) and the solution stirred at 50° C. for 3 h. The reaction mixture was cooled in an ice bath then acidified by the addition of 1 N HCl (20 mL). The resulting precipitate was filtered, rinsed with water then dried under vacuum to give Compound 46a (790 mg, 89% yield) as a white solid. LCMS ESI 277.0 (M+H), RT=1.41 min (Method Q). 1H NMR (400 MHz, DMSO-d6) δ 13.49 (br. s., 1H), 12.91 (br. s., 1H), 7.90-6.67 (m, 5H), 5.01 (s, 2H), 3.86 (s, 3H).

1. temperatureThe reaction mixture was cooled in an ice bath
2. filtrationThe resulting precipitate was filtered
3. washrinsed with water
4. customthen dried under vacuum