反应详情

In a 25-mL round-bottom flask, the benzyl 4-(2-chloroacetyl)morpholine-2-carboxylate (0.262 g, 0.88 mmol) was dissolved in dmf (4 mL). Sodium azide (0.066 g, 1.0 mmol) was added, and the flask was placed in a 60 deg oil bath overnight. The reaction was concentrated, and the residue was taken up in 80% ether-hexane (60 mL) and the organic layer was extracted with dilute sodium bicarbonate (2×7 mL) then with saturated brine (7 mL), then was dried over magnesium sulfate, filtered, and concentrated. The residue was purified through silica gel (50 mL) which had been deactivated with TEA (5 mL) using 60% EtOAc-hexane to afford the title compound (230 mg, 0.76 mmol). MS m/z 305 (M+1).

1. customwas placed in a 60 deg
2. customovernight
3. concentrationThe reaction was concentrated
4. extractionthe organic layer was extracted with dilute sodium bicarbonate (2×7 mL)
5. dry with materialwith saturated brine (7 mL), then was dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified through silica gel (50 mL) which