HRID2105890

反应详情

EQUATION

反应方程式

HRID 2105890 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

AlCl3 (12.1 g) was added to a solution of N-biphenyl-2-yl-2-chloro-acetamide (9.9 g) in 1,3-dichlorobenzene (99 mL). The reaction mixture was stirred for 24 hours at 170° C., cooled to 0° C. and poured into ice-water (1500 mL). The suspension obtained was filtered off, the precipitate washed with water (250 mL), 2 portions of hexane/dichloromethane 4:1 (25 mL), 2 portions of water (125 mL) and 2 portions of hexane (25 mL) affording 5H,7H-dibenzo[b,d]azepin-6-one (6.9 g, 82.5%) as an off-white powder.

WORKUP

后处理

  1. temperaturecooled to 0° C.
  2. customThe suspension obtained
  3. filtrationwas filtered off
  4. washthe precipitate washed with water (250 mL), 2 portions of hexane/dichloromethane 4:1 (25 mL), 2 portions of water (125 mL) and 2 portions of hexane (25 mL)