HRID1168457

反应详情

EQUATION

反应方程式

HRID 1168457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

2-Phenylbutane-1,2-diamine (328 mg, 2.0 mmol) in 4.4 mL of toluene is added dropwise to a stirred solution of trimethylaluminum (2.0 M, 1 mL) in 5 mL of toluene at below 10° C. under nitrogen. At the end of methane evolution, methyl-2-phenyl-4-quinolinecarboxylate (263 mg, 1 mmol) in 2 mL of toluene is gradually added at room temperature. The reaction mixture is refluxed for 3 hours under nitrogen. After cooling, the solution is treated with 1 mL of water, diluted with 1 mL of methanol and 1 mL of methylene chloride, and refluxed for 15 minutes. After separation of organic solvent and solvent evaporation, the residue is purified over silica gel chromatography eluting with 5-10% MeOH/CH2Cl2. The corresponding compound is obtained as a white solid.

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 3 hours under nitrogen
  2. temperatureAfter cooling
  3. temperaturerefluxed for 15 minutes
  4. customAfter separation of organic solvent and solvent evaporation
  5. customthe residue is purified over silica gel chromatography
  6. washeluting with 5-10% MeOH/CH2Cl2
  7. customThe corresponding compound is obtained as a white solid