HRID1174683
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
In a Parr bottle, a mixture of 2-amino-3-quinolin-5-yl-butyronitrile (Intermediate-E2) (5.38 g, 25.4 mmol) in MeOH (100 mL) and ethylene diamine (3.2 mL, 47.8 mmol) was reacted with Raney 2800 nickel (18.9 g) and bubbled with ammonia gas for 10 m. The Parr bottle was pressurized with hydrogen at 50 psi and shaken on a Parr apparatus for 2.5 h at rt. The mixture was filtered through celite, washed with MeOH (3×) and evaporated to leave a residue. This material was placed onto a column and eluted with a gradient of 1% to 5% sat. NH3-MeOH:CH2Cl2 to give 3-quinolin-5-yl-butane-1,2-diamine (Intermediate E3) 3.9 g (71%).
WORKUP
后处理
- custombubbled with ammonia gas for 10 m
- filtrationThe mixture was filtered through celite
- washwashed with MeOH (3×)
- customevaporated
- customto leave a residue
- washeluted with a gradient of 1% to 5% sat. NH3-MeOH