HRID1910399
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
To a solution of tert-butyl [(2R)-2-methoxypropyl]carbamate (2.72 g) in DMF (41 ml) was added NaH (862 mg; 60% oil suspension) under nitrogen atmosphere, and the mixture was stirred at room temperature for 30 minutes. MeI (1.79 ml) was added to the mixture, and the whole was stirred for 3 hours at the same temperature. Water was added, and the whole was extracted with EtOAc and the extract was washed with water and brine and dried over MgSO4. Concentration under reduced pressure gave a residual oil, which was purified with silica gel column eluting with EtOAc:n-hexane=1:5 to give tert-butyl [(2R)-2-methoxypropyl]methylcarbamate (1.94 g).
WORKUP
后处理
- stirringthe whole was stirred for 3 hours at the same temperature
- extractionthe whole was extracted with EtOAc
- washthe extract was washed with water and brine
- dry with materialdried over MgSO4
- concentrationConcentration under reduced pressure
- customgave a residual oil, which
- customwas purified with silica gel column
- washeluting with EtOAc