HRID351571

反应详情

EQUATION

反应方程式

HRID 351571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

To a solution of 5,6-Dihydro-4H-pyrrolo[3,2,1-ij]quinoline-1-carboxylic acid ethyl ester (31 g, 0.14 mol) in ethanol (200 mL) and water (70 mL) was added 5 N aqueous sodium hydroxide(60 mL, 0.3 mol) and the resulting mixture stirred at reflux for 3 hours. The reaction mixture was cooled to 20-24° C., diluted with water (2 L) and washed with dichloromethane(2×200 mL) and diethyl ether (1×200 mL). The aqueous layer was filtered through Celite and the filtrate was acidified with conc. HCl (25 mL) to precipitate the product. The solid was filtered, washed with water (200 mL), and dried in vacuo to give 23.2 g (85%) of the desired compound as a light yellow solid.

WORKUP

后处理

  1. temperatureat reflux for 3 hours
  2. washwashed with dichloromethane(2×200 mL) and diethyl ether (1×200 mL)
  3. filtrationThe aqueous layer was filtered through Celite
  4. customto precipitate the product
  5. filtrationThe solid was filtered
  6. washwashed with water (200 mL)
  7. customdried in vacuo