HRID1910399

反应详情

EQUATION

反应方程式

HRID 1910399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringthe whole was stirred for 3 hours at the same temperature
  2. extractionthe whole was extracted with EtOAc
  3. washthe extract was washed with water and brine
  4. dry with materialdried over MgSO4
  5. concentrationConcentration under reduced pressure
  6. customgave a residual oil, which
  7. customwas purified with silica gel column
  8. washeluting with EtOAc