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
2,3-Lutidine (321 g) was added with stirring to a solution of sodamide (351 g) in liquid ammonia (3 1). 1-Amino-3-chloropropane hydrochloride (429g) was added to this mixture over 8 minutes with stirring. Any liquid ammonia lost through evaporation was replaced. After 2 hours the reaction was quenched by the addition of ammonium chloride (120 g) and the reaction mixture was left to stand overnight to allow substantially complete escape of ammonia through evaporation. The residue so obtained was diluted with water (2 1) and extracted with dichloromethane. The extracts were dried (Na2SO4), the dichloromethane removed by evaporation and the residue distilled in vacuo to give 4-(3-methyl-2-pyridyl) butylamine (306.6 g).
WORKUP
后处理
- customAny liquid ammonia lost through evaporation
- customAfter 2 hours the reaction was quenched by the addition of ammonium chloride (120 g)
- waitthe reaction mixture was left
- customthrough evaporation
- customThe residue so obtained
- extractionextracted with dichloromethane
- dry with materialThe extracts were dried (Na2SO4)
- customthe dichloromethane removed by evaporation
- distillationthe residue distilled in vacuo