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
tert-Butyl 1-oxo-4-phenyl-2,7-diazaspiro[4,5]decane-7-carboxylate (ASW MedChem) (1 g, 3.03 mmol) was dissolved in THF (20 ml) under an atmosphere of nitrogen. The solution was cooled (ice/brine bath) and treated with sodium hydride (60% in oil) (0.133 g, 3.33 mmol). The reaction mixture was stirred for 10 minutes and iodoethane (0.269 ml, 3.33 mmol) was added dropwise. The ice bath was removed and the reaction mixture was stirred at room temperature overnight. The reaction was quenched with water and extracted with ethyl acetate. The organic phase was washed with brine, dried (MgSO4) and concentrated in vacuo to afford the title compound. The resulting diastereomeric mixture was used in the next step without further purification.
WORKUP
后处理
- customThe ice bath was removed
- stirringthe reaction mixture was stirred at room temperature overnight
- customThe reaction was quenched with water
- extractionextracted with ethyl acetate
- washThe organic phase was washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo