HRID467413

反应详情

EQUATION

反应方程式

HRID 467413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Propane-2-yl-benzene (100 mmol), acetic acid palladium (2.7 mmol), triphenylphosphine (5 mmol), and sodium carbonate (50 mmol) were put in a dried two-neck round-bottom flask and dissolved in DMF (100 ml). Subsequently, tert-butyl-(2-iodo-benzylidene)amine (50 mmol) was added thereto. The resulting solution was stirred in a bath at 100° C. for 24 hours. After completion of the reaction, the temperature was allowed to cool to room temperature. The reaction mixture was extracted with ether and saturated NH4Cl. The extract was distilled under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane: EtOAc=5:1) to yield 3-(3,5-dimethylphenyl)-4-methylisoquinoline.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. temperatureto cool to room temperature
  3. extractionThe reaction mixture was extracted with ether and saturated NH4Cl
  4. distillationThe extract was distilled under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (hexane: EtOAc=5:1)