HRID23951

反应详情

EQUATION

反应方程式

HRID 23951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

1-t-Butoxycarbonyl-4-piperidinol (5.0 g 24.88 mmol) in dry dimethylformamide (60 ml) was treated with sodium hydride (60% 2.99 g 74.75 mmol) at room temperature under argon and then with 2-chloropyridine hydrochloride (4.1 g 27.33 mmol). Then mixture was heated at 80° C. overnight. After cooling the reaction was carefully quenched with water (5 ml) and then diluted with more water (20 ml) and extracted with ethyl acetate (30 ml). The organic solution was washed with sat. sodium bicarbonate, dried (MgSO4) and evaporated to give 1-t-butoxycarbonyl-4-(2-pyridoxy)piperidine (4.96 g 72%).

WORKUP

后处理

  1. temperatureAfter cooling the reaction
  2. customwas carefully quenched with water (5 ml)
  3. additiondiluted with more water (20 ml)
  4. extractionextracted with ethyl acetate (30 ml)
  5. washThe organic solution was washed with sat. sodium bicarbonate
  6. dry with materialdried (MgSO4)
  7. customevaporated