HRID1815061
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
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 the 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 satd sodium bicarbonate, dried (MgSO4) and evaporated to give 1-t-butoxycarbonyl-4-(2-pyridoxy)piperidine (4.96 g, 72%).
WORKUP
后处理
- temperatureAfter cooling
- customthe reaction was carefully quenched with water (5 mL)
- additiondiluted with more water (20 mL)
- extractionextracted with ethyl acetate (30 mL)
- washThe organic solution was washed with satd sodium bicarbonate
- dry with materialdried (MgSO4)
- customevaporated