HRID565688

反应详情

EQUATION

反应方程式

HRID 565688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

In an autoclave, a mixture of 2-bromomethyl-2,3-dihydro-2,4,6,7-tetramethyl-5-benzofuranamine (0.85 g), 4-benzylpiperidine (1.1 g), and triethylamine (1.3 mL) was stirred under nitrogen gas at 180° C. for 15 hours. This reaction mixture was diluted with saturated aqueous NaHCO3 and extracted with 2 portions of ethyl acetate. The pooled organic layer was washed with water and saturated aqueous NaCl and dried over MgSO4. After filtration, the filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (hexane/ethanol=10:1) and crystallized from hexane to provide 0.86 g of the title compound. Yield 78%.

WORKUP

后处理

  1. extractionextracted with 2 portions of ethyl acetate
  2. washThe pooled organic layer was washed with water and saturated aqueous NaCl
  3. dry with materialdried over MgSO4
  4. filtrationAfter filtration
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customcrystallized from hexane