反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 30 °C
PROCEDURE
实验过程
A mixture of 119b (150 mg, 0.26 mmol) and lithium hydroxide (61.4 mg, 2.6 mmol) in i-propanol/THF (1:1, 4 mL) and water (1 mL) was stirred at 30° C. for 1 h. The mixture was evaporated in vacuo and the residue was diluted with water (5 mL). It was then extracted with ethyl acetate (2×10 mL). The combined ethyl acetate extract was concentrated under reduced pressure and the residue was purified by reverse-phase prep-HPLC to afford 119 (75.0 mg, 54%) as a white solid. MS-ESI: [M+H]+ 544.3. 1H NMR (500 MHz, CDCl3) δ 8.66 (d, J=5.0 Hz, 1H), 8.35 (d, J=2.0 Hz, 1H), 7.97 (d, J=2.0 Hz, 1H), 7.59-7.53 (m, 4H), 7.37 (s, 1H), 5.74 (s, 1H), 4.51 (s, 2H), 4.07 (s, 1H), 3.72 (s, 3H), 3.70 (s, 3H), 2.25 (s, 3H), 1.46 (s, 9H).
WORKUP
后处理
- customThe mixture was evaporated in vacuo
- additionthe residue was diluted with water (5 mL)
- extractionIt was then extracted with ethyl acetate (2×10 mL)
- extractionThe combined ethyl acetate extract
- concentrationwas concentrated under reduced pressure
- customthe residue was purified by reverse-phase prep-HPLC