HRID1589402

反应详情

EQUATION

反应方程式

HRID 1589402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe solution was cooled
  2. customthe aqueous layer was then decanted from the red coloured oil which
  3. washwas washed with more water
  4. washThe oil was subjected to chromatography on silica gel using gradient elution (100% chloroform→2% Methanol in chloroform)
  5. additionThe fractions containing the desired product
  6. customwere collected
  7. customevaporated under reduced pressure