反应详情

NaH (70%, 0.504 g, 15 mmol) was added in portions to a solution of (S)-tert-butyl 1-cyclopropyl-3-hydroxypropan-2-ylcarbamate (1.6 g, 7.5 mmol) in THF (30 mL) at room temperature. The mixture was stirred at room temperature for 20 min. 1-Bromo-2-methoxyethane (2.07 g, 15 mmol) was added and stirring was continued for 2 h. The reaction was quenched by careful addition of H2O (5 mL). After evaporation of solvent the residue was diluted with ethyl acetate (20 mL) and H2O (20 mL). The organic layer was washed with brine (20 mL), dried over Na2SO4, and concentrated to give the title product as yellow oil (1.01 g, 50%); MS (EI): m/e=296.2 [M+Na]+.

1. stirringstirring
2. waitwas continued for 2 h
3. customThe reaction was quenched by careful addition of H2O (5 mL)
4. customAfter evaporation of solvent the residue
5. additionwas diluted with ethyl acetate (20 mL) and H2O (20 mL)
6. washThe organic layer was washed with brine (20 mL)
7. dry with materialdried over Na2SO4
8. concentrationconcentrated