HRID920769
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
- 80 °C
PROCEDURE
实验过程
To a stirred solution of Intermediate 285B (1.5 g, 5.85 mmol) in ethanol (20 ml) was added a solution of KOH (1.313 g, 23.41 mmol) in water (10 mL). The resulting solution was stirred at 80° C. for 16 h. The reaction mixture was cooled to RT, quenched with crushed ice and extracted with diethyl ether (2×50 mL). The combined organic layers were dried over Na2SO4 and evaporated to afford Intermediate 285C as a viscous liquid (0.9 g, 89% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 12.64 (br. s., 2H), 2.17-2.29 (m, 4H), 1.01-1.12 (m, 6H).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to RT
- customquenched with crushed ice
- extractionextracted with diethyl ether (2×50 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- customevaporated