HRID2104600

反应详情

EQUATION

反应方程式

HRID 2104600 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(2-Fluorophenyl)-3-oxopropionaldehyde (0.451 g, 2.70 mmol) and [2-amino-3-(trifluoromethyl)phenyl](phenyl)methanone (0.119 g, 0.448 mmol) in AcOH (5 mL) is treated with 0.1 mL of 1:20H2SO4/AcOH solution and heated at reflux for 20 min. The cooled reaction is quenched with water and extracted with ethyl acetate twice. The combined organic layers are washed with saturated aq sodium bicarbonate and dried over MgSO4. The product is purified by chromatography (5:95 ethyl acetate:hexane) to afford the title compound as a yellow solid (0.162 g, 91.5%). MS (ESI) m/z 396.1009; HRMS: calcd for C23H13F4NO+H, 396.10115; found (ESI, [M+H]+), 396.1009.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 20 min
  3. customThe cooled reaction
  4. customis quenched with water
  5. extractionextracted with ethyl acetate twice
  6. washThe combined organic layers are washed with saturated aq sodium bicarbonate
  7. dry with materialdried over MgSO4
  8. customThe product is purified by chromatography (5:95 ethyl acetate:hexane)