HRID1783777
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
PROCEDURE
实验过程
To a solution of 1-(3-butyl-imidazo[1,5-a]pyridin-1-yl)-2,2,2-trifluoro-ethanone (400 mg, 1.48 mmol) in EtOH (10 mL) was added KOH (830 mg, 14.8 mmol). The mixture was stirred at ambient temperature for 15 h. After this time the mixture was concentrated, diluted with water (10 mL) and acidified to pH 3 with 2N HCl. The aqueous mixture was extracted with ethyl acetate (3×50 mL) and the combined organic layers were dried over anhydrous sodium sulfate and concentrated in vacuo to yield the title compound (200 mg, 62%). 1H NMR (DMSO-d6) δ 12.1 (1H), 8.38 (1H), 7.99 (1H), 7.18 (1H), 6.90 (1H), 2.99 (2H), 1.75 (2H), 1.38 (2H), 0.92 (3H); m/z (M+H)=219.0.
WORKUP
后处理
- concentrationAfter this time the mixture was concentrated
- additiondiluted with water (10 mL)
- extractionThe aqueous mixture was extracted with ethyl acetate (3×50 mL)
- dry with materialthe combined organic layers were dried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo