HRID24923

反应详情

EQUATION

反应方程式

HRID 24923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2.5 g (11.1 mmol) of tin dichloride dihydrate are added at ambient temperature to a solution of 1.5 g (6.46 mmol) of 4-[2-(3,6-dihydro-2H-pyridin-1-yl)-ethyl]-nitrobenzene, prepared analogously to Example 254, in 7 ml of glacial acetic acid and 2.5 ml of concentrated hydrochloric acid. The mixture is heated for 4 hours to 100° C., then another 2.5 g (11.1 mmol) of tin dichloride dihydrate are added and the mixture is heated for 12 hours to 100° C. After cooling the solvent is eliminated in vacuo and the residue taken up in water. The mixture is made alkaline with 4N sodium hydroxide solution and extracted with dichloromethane. After removal of the solvent in vacuo the product is obtained as an oil.

WORKUP

后处理

  1. temperatureThe mixture is heated for 4 hours to 100° C.
  2. temperaturethe mixture is heated for 12 hours to 100° C
  3. temperatureAfter cooling the solvent
  4. extractionextracted with dichloromethane
  5. customAfter removal of the solvent in vacuo the product
  6. customis obtained as an oil