HRID1599426

反应详情

EQUATION

反应方程式

HRID 1599426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureto reflux for 2 h
  2. temperatureThe reaction mixture was cooled to room temperature
  3. customquenched with water
  4. filtrationfiltered
  5. customThe solvent was evaporated in vacuo
  6. dissolutionthe residue dissolved in 20% sulphuric acid
  7. filtrationThe precipitate was filtered off
  8. additionthe liquid phase added potassium hydroxide to pH 11
  9. customThe product was isolated by continuous liquid/liquid extraction (ethyl acetate) overnight