HRID1088702
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- distillationdistilled under vacuum
- customto remove benzylamine
- customThe residue was partitioned between ethyl acetate (300 ml) and 8% aqueous sodium bicarbonate (200 ml)
- concentrationThe dried organic layer was concentrated
- customthe residual oil was purified by FCC
- washeluting with ethyl acetate-triethylamine (100:1)