HRID1649427

反应详情

EQUATION

反应方程式

HRID 1649427 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 50 ml of concentrated hydrochloric acid having dissolved therein 25 g of stannous chloride was added 6.7 g of 5-nitro-6-chloroquinaldine and the mixture was allowed to react on a water bath at a temperature of 80° to 90° C. for 30 minutes. The reaction mixture was ice-cooled, rendered alkaline (pH 10) with 30% sodium hydroxide and filtered and extracted with 500 ml of chloroform and Celite (diatomaceous earth). After drying over anhydrous sodium sulfate the chloroform fraction was concentrated and recrystallized from a mixture of benzene and hexane to obtain 4.5 g of 5-amino-6-chloroquinaldine as colorless plates having a melting point of 196° to 197° C.

WORKUP

后处理

  1. customto react on a water bath at a temperature of 80° to 90° C. for 30 minutes
  2. temperaturecooled
  3. filtrationfiltered
  4. extractionextracted with 500 ml of chloroform and Celite (diatomaceous earth)
  5. dry with materialAfter drying over anhydrous sodium sulfate the chloroform fraction
  6. concentrationwas concentrated
  7. customrecrystallized from a mixture of benzene and hexane