反应详情

To a round bottom flask charged with (+/−)-tert-butyl 2-(hydroxymethyl)morpholine-4-carboxylate (2 g, 9.21 mmol) in DMF (2 mL) was added imidazole and TBS-Cl (1.387 g, 9.21 mmol). The reaction mixture was stirred at room temperature 2 d. The reaction mixture was poured into a separatory funnel containing half-saturated aqueous ammonium chloride and ether. The aqueous layer was extracted with ether (2×). The combined organics were washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. (+/−)-tert-Butyl 2-(((tert-butyldimethylsilyl)oxy)methyl)morpholine-4-carboxylate (3.039 g) was isolated as a white pasty solid.

1. additionThe reaction mixture was poured into a separatory funnel
2. extractionThe aqueous layer was extracted with ether (2×)
3. washThe combined organics were washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo