HRID11563

反应详情

EQUATION

反应方程式

HRID 11563 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

A room temperature solution of 1.1180 gms. 4-(4-nitro-phenyl)-butyric acid in tetrahydrofuran (3 mL) is treated with 0.9052 gms. 1′,1′-carbonyl-diimidizole using an ice bath to attenuate the intensity of the reaction. The reaction mixture is stirred for 1 h. The reaction mixture is then treated with 0.5 mL morpholine. The reaction is heated overnight at 35° C. The reaction is then allowed to cool to room temperature, and is made basic with the addition of saturated aqueous sodium bicarbonate. The resulting mixture is extracted with ethyl acetate. The organics are dried over anhydrous sodium sulfate, filtered and evaporated to dryness in vacuo. The crude product residue is then chromatographed by flash silica gel chromatography using 60% ethyl acetate in hexanes as the eluant. Following evaporation of solvent, 1-morpholin-4-yl-4-(4-nitro-phenyl)-butan-1-one is isolated as a white solid in the amount of 1.3925 gms.

WORKUP

后处理

  1. customA room temperature solution of 1.1180 gms
  2. customthe intensity of the reaction
  3. temperatureto cool to room temperature
  4. extractionThe resulting mixture is extracted with ethyl acetate
  5. dry with materialThe organics are dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness in vacuo
  8. customThe crude product residue is then chromatographed by flash silica gel chromatography
  9. customevaporation of solvent