HRID1048913

反应详情

EQUATION

反应方程式

HRID 1048913 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

5.34 g of N-(2-butyl-1-benzofuran-5-yl)methanesulfonamide (II) (0.02 mol, 1 eq) is dissolved in 40 mL of trifluoroacetic acid and 8.7 g of 4-(3-dibutylamino-propoxy)-benzaldehyde (V) (0.03 mol, 1.5 eq) is added to the solution. The reaction mixture is heated to 40° C. and stirred for 10 hours at this temperature. The mixture is cooled to room temperature and 100 mL of water is added. After 15 min of stirring, the product is extracted with 2×50 mL of dichloromethane. The organic phase is concentrated and the crude product is purified by column chromatography (spheric silica; eluent:toluene:MTBE:methanol=50:40:10) to obtain 3.68 g of compound (VI) (33%).

WORKUP

后处理

  1. temperatureThe mixture is cooled to room temperature
  2. stirringAfter 15 min of stirring
  3. extractionthe product is extracted with 2×50 mL of dichloromethane
  4. concentrationThe organic phase is concentrated
  5. customthe crude product is purified by column chromatography (spheric silica; eluent:toluene:MTBE:methanol=50:40:10)