反应详情

To a solution of azocane (5.59 g, 49.4 mmol) and triethylamine (6.53 g, 64.7 mmol) in DCM (50 mL) at room temperature was added (2-bromoethoxy)(tert-butyl)dimethylsilane (13.0 g, 54.4 mmol). The mixture was stirred overnight, and the solvent was removed under reduced pressure. The residue was dissolved in ethyl acetate, washed (brine (2×)), dried over Na2SO4 and filtered. The solvent was removed under reduced pressure, and the residue was purified on a silica gel column (eluting with PE/EA=10/1) to afford 1-(2-((tert-butyldimethylsilyl)oxy)ethyl)azocane (11.8 g, 88%). LCMS: 272 (M+H)+.

1. customthe solvent was removed under reduced pressure
2. dissolutionThe residue was dissolved in ethyl acetate
3. washwashed (brine (2×))
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customThe solvent was removed under reduced pressure
7. customthe residue was purified on a silica gel column (eluting with PE/EA=10/1)