HRID612073

反应详情

EQUATION

反应方程式

HRID 612073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6.30 g (19.4 mmol) 4-[(3-chlorophenyl)amino]-6-nitro-3-quinolinecarbonitrile, 300 ml ethanol, and 21.9 g (97 mmol) SnCl2 dihydrate were heated to reflux under N2. Removed heat at 2.5 hours, added ice water and made basic with sodium bicarbonate. Stirred for 2 hours and extracted with chloroform. Dried organic layer with sodium sulfate, filtered, stripped solvent and dried residue in vacuo, giving 5.74 g of yellow-brown solid: mass spectrum (electrospray m/e): M+H=295.1, 297.1.

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureto reflux under N2
  3. customRemoved
  4. temperatureheat at 2.5 hours
  5. additionadded ice water
  6. extractionextracted with chloroform
  7. filtrationDried organic layer with sodium sulfate, filtered