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 a solution of 2-methyl-4-phenylimino-3,4-dihydro-2H-quinoline-1-carboxylic acid benzyl ester (16 g) in acetic acid (450 ml), sodium triacetoxyborohydride was added in small amounts (32.32 g), under stirring, at room temperature. The reaction mixture was then stirred at room temperature for one hour and poured on 1 liter of cold water under stirring. After precipitation, the mixture was filtered, dissolved in ethyl acetate and then, washed with water. The organic layer was separated and dried over sodium sulfate. The solvent was removed to give the crude compound (9g), recristallised in hot cyclohexane (40 ml), and then filtered at room temperature to give the desired compound (5.3 g, 46.6% yield).
WORKUP
后处理
- stirringThe reaction mixture was then stirred at room temperature for one hour
- stirringunder stirring
- customAfter precipitation
- filtrationthe mixture was filtered
- dissolutiondissolved in ethyl acetate
- washwashed with water
- customThe organic layer was separated
- dry with materialdried over sodium sulfate
- customThe solvent was removed
- customto give the crude compound (9g)
- filtrationfiltered at room temperature