HRID1088702

反应详情

EQUATION

反应方程式

HRID 1088702 的结构方程式

PROCEDURE

实验过程

2-[6-[(6-Bromohexyl)oxy]hexyl]pyridine (4.99 g) was added dropwise to benzylamine (22 ml) at 140° C. under nitrogen. The solution was stirred at 140° for 1 h and distilled under vacuum to remove benzylamine. The residue was partitioned between ethyl acetate (300 ml) and 8% aqueous sodium bicarbonate (200 ml). The dried organic layer was concentrated and the residual oil was purified by FCC eluting with ethyl acetate-triethylamine (100:1) to give the title compound as a pale yellow oil (4.65 g), t.l.c. (ethyl acetate+few drops triethylamine) Rf 0.23.

WORKUP

后处理

  1. distillationdistilled under vacuum
  2. customto remove benzylamine
  3. customThe residue was partitioned between ethyl acetate (300 ml) and 8% aqueous sodium bicarbonate (200 ml)
  4. concentrationThe dried organic layer was concentrated
  5. customthe residual oil was purified by FCC
  6. washeluting with ethyl acetate-triethylamine (100:1)