HRID747275

反应详情

EQUATION

反应方程式

HRID 747275 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. custombubbled with ammonia gas for 10 m
  2. filtrationThe mixture was filtered through celite
  3. washwashed with MeOH (3×)
  4. customevaporated
  5. customto leave a residue
  6. washeluted with a gradient of 1% to 5% sat. NH3-MeOH