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
- 25 °C
PROCEDURE
实验过程
To a suspension of lithium aluminium hydride (400 mg, 10.5 mmol) in dry tetrahydrofuran (200 ml) was added 2-ethoxycarbonyl-1-(1-imidazolylmethyl)-7-trifluoromethylimidazo[1,2-a]quinoxalin-4(5H)-one (3.6 g, 8.8 mmol) in small portions. After 20 min. at 25° C. the temperature was raised to reflux for 2 h. The reaction mixture was cooled to room temperature, quenched with water and then filtered, The solvent was evaporated in vacuo and the residue dissolved in 20% sulphuric acid. The precipitate was filtered off and the liquid phase added potassium hydroxide to pH 11. The product was isolated by continuous liquid/liquid extraction (ethyl acetate) overnight to give 2.1 g (67%) of the title compound. M.p. 215° C.
WORKUP
后处理
- temperatureto reflux for 2 h
- temperatureThe reaction mixture was cooled to room temperature
- customquenched with water
- filtrationfiltered
- customThe solvent was evaporated in vacuo
- dissolutionthe residue dissolved in 20% sulphuric acid
- filtrationThe precipitate was filtered off
- additionthe liquid phase added potassium hydroxide to pH 11
- customThe product was isolated by continuous liquid/liquid extraction (ethyl acetate) overnight