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
- 50 °C
PROCEDURE
实验过程
To a solution of ethyl 3-[5-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1H-indazol-1-yl]-2,2-dimethylpropanoate (D100) (85 mg, 176 mmol) in THF (2 ml) at room temperature was added NaOH (2N in H2O, 440 μl, 880 mmol) and the resulting mixture was stirred at 50° C. overnight. NaOH (2N in H2O, 440 μl, 880 mmol) and THF (2 ml) were added and the resulting mixture stirred at 80° C. for two nights then cooled to room temperature. Most of THF was removed in vacuo and the resulting aqueous phase was acidified to pH 3. The precipitate formed was filtered off and washed with H2O then dried at 60° C. under vacuum to give the title compound (73 mg, 91%) as a white solid. MS (ES): C23H23ClN4O4 requires 454; found (MH+) 455.
WORKUP
后处理
- stirringthe resulting mixture stirred at 80° C. for two nights
- temperaturethen cooled to room temperature
- customMost of THF was removed in vacuo
- customThe precipitate formed
- filtrationwas filtered off
- washwashed with H2O
- customthen dried at 60° C. under vacuum