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-[[4-(3-Methoxy-2-pyridyl)butyl]amino]-4-(1H)-pyrimidinone (0.14 g) and pyridine-4-aldehyde (0.06 g) were refluxed in concentrated hydrochloric acid (1 ml) for 5 hours. The solution was cooled and neutralised by the addition of potassium bicarbonate. Water (2 ml) was added, the aqueous layer was then decanted from the red coloured oil which was washed with more water. The oil was subjected to chromatography on silica gel using gradient elution (100% chloroform→2% Methanol in chloroform). The fractions containing the desired product were collected, combined and evaporated under reduced pressure to afford the title compound as an oil; δ(CDCl3) 1.67 (4H, m), 2.80 (2H, t), 3.36 (2H, m), 3.80 (3H, s), 5.72 (1H, s), 7.07 (2H, d), 7.35 (2H, d), 7.49 (1H, s), 7.87 (1H, t), 8.43 (2H, m) ppm.
WORKUP
后处理
- temperatureThe solution was cooled
- customthe aqueous layer was then decanted from the red coloured oil which
- washwas washed with more water
- washThe oil was subjected to chromatography on silica gel using gradient elution (100% chloroform→2% Methanol in chloroform)
- additionThe fractions containing the desired product
- customwere collected
- customevaporated under reduced pressure