HRID1091794
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
- 40 °C
PROCEDURE
实验过程
Tert-butyl 4-(2-oxo-2-(piperidin-1-yl)ethoxy)piperidine-1-carboxylate (111) (7.5 g, 22.98 mmol) was dissolved in dry THF (100 mL), to this was added borane-methyl sulfide complex (17.23 mL, 34.46 mmol) and the reaction was stirred at 40° C. for 3 hours then at ambient temperature overnight. The gummy mixture was evaporated and was quenched with 2.0 N sodium carbonate (50 mL), extracted with EtOAc (3×75 mL), the organic layer was dried over MgSO4, filtered and evaporated to afford tert-butyl 4-(2-(piperidin-1-yl)ethoxy)piperidine-1-carboxylate (7.3 g, 95% yield) as a colourless liquid and used without further purification.
WORKUP
后处理
- additionto this was added borane-methyl sulfide complex (17.23 mL, 34.46 mmol)
- customat ambient temperature
- customovernight
- customThe gummy mixture was evaporated
- customwas quenched with 2.0 N sodium carbonate (50 mL)
- extractionextracted with EtOAc (3×75 mL)
- dry with materialthe organic layer was dried over MgSO4
- filtrationfiltered
- customevaporated