反应详情

To a solution of the compound obtained in Step C (3.52 g/14.65 mmol) in 50 ml of 1,2-dichloroethane there are added dropwise trimethylsilyl azide (TMSN3), and then 0.326 g (1.46 mmol) of magnesium perchlorate (Mg(ClO4)2), and the whole is stirred at room temperature overnight. Hydrolysis is then carried out using H2O, followed by extraction with AcOEt; the organic phases are then combined, washed with a saturated NaCl solution, dried over MgSO4 and concentrated to dryness. The yellow oil so obtained is chromatographed over a column of silica gel (cyclohexane, 2% AcOEt) to yield the title product in the form of a translucent oil.

1. customHydrolysis
2. extractionfollowed by extraction with AcOEt
3. washwashed with a saturated NaCl solution
4. dry with materialdried over MgSO4
5. concentrationconcentrated to dryness
6. customThe yellow oil so obtained
7. customis chromatographed over a column of silica gel (cyclohexane, 2% AcOEt)