HRID1402647

反应详情

EQUATION

反应方程式

HRID 1402647 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1-(4-carbazol-9-yl-phenyl)ethanone (30.0 g) in CH2Cl2 (1200 mL) is added thiophenecarbonyl chloride (15.4 g) and AlCl3 (28.4 g) at 0° C. After stirring overnight at room temperature, crotonyl chloride (11.3 g) and AlCl3 (15.5 g) are further added at 0° C. and the mixture is stirred at room temperature overnight. The reaction mixture is poured into ice-water, and the crude product is extracted twice with CH2Cl2. The combined organic layer is washed with H2O and brine, dried over MgSO4, and concentrated to give the residue, which is purified by washing with hot ethyl acetate.

WORKUP

后处理

  1. stirringthe mixture is stirred at room temperature overnight
  2. extractionthe crude product is extracted twice with CH2Cl2
  3. washThe combined organic layer is washed with H2O and brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customto give the residue, which
  7. customis purified
  8. washby washing with hot ethyl acetate