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