HRID1167718
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 1-(3-aminopropyl)-4-(pyrid-2-yl]pyridinium bromide hydrobromide (0.66 g, 1.75 mmol) in 20.0 mL MeOH was added NaBH4 (0.101 g, 2.62 mmol) in small portions. The reaction mixture was stirred for 30 min and then quenched with 6M HCl solution. The solution was concentrated to 20.0 mL and basified with 50% NaOH solution to pH 12. Extracted with CHCl3 (5×30.0 mL), dried over MgSO4 and the solvent was removed to give 3-(3′,6′-dihydro-2′-H-[2,4′]bipyridinyl-1′-yl)-propylamine as an oil (0.37 g, 96% yield). It is used in the next step immediately without purification.
WORKUP
后处理
- customquenched with 6M HCl solution
- concentrationThe solution was concentrated to 20.0 mL and basified with 50% NaOH solution to pH 12
- extractionExtracted with CHCl3 (5×30.0 mL)
- dry with materialdried over MgSO4
- customthe solvent was removed