HRID877520

反应详情

EQUATION

反应方程式

HRID 877520 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-benzylidene-6,7-dichloro-2,3,4,9-tetrahydro-1H-carbazol-1-one (0.07 g, 0.20 mmol) in EtOAc (10 mL), 10% Pd/C (10 mg) was added under N2 atmosphere. The reaction mixture was stirred under H2 atmosphere at room temperature for 12 h. The reaction mixture was filtered through a Celite® pad. The Celite® pad was washed with EtOAc (2×20 mL) and the filtrate was concentrated in vacuo to provide the crude material which was purified by silica gel chromatography [EtOAc-hexane (1:9) as eluant] to furnish the title compound as a yellow solid (0.04 g, 57%). 1H NMR (500 MHz, CDCl3, δ in ppm) 8.79 (s, 1H), 7.73 (s, 1H), 7.54 (s, 1H), 7.34-7.31 (m, 2H), 7.25-7.22 (m, 3H), 3.48-3.45 (m, 1H), 3.02-2.97 (m, 1H), 2.86-2.81 (m, 2H), 2.80-2.66 (m, 1H), 2.25-2.21 (m, 1H), 1.95-1.92 (m, 1H).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through a Celite® pad
  2. washThe Celite® pad was washed with EtOAc (2×20 mL)
  3. concentrationthe filtrate was concentrated in vacuo
  4. customto provide the crude material which
  5. customwas purified by silica gel chromatography [EtOAc-hexane (1:9) as eluant]