HRID1649427
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customto react on a water bath at a temperature of 80° to 90° C. for 30 minutes
- temperaturecooled
- filtrationfiltered
- extractionextracted with 500 ml of chloroform and Celite (diatomaceous earth)
- dry with materialAfter drying over anhydrous sodium sulfate the chloroform fraction
- concentrationwas concentrated
- customrecrystallized from a mixture of benzene and hexane