反应详情

To a stirred solution of [(3S,6R)-6-(6-azido-hexyloxy)-1-methyl-2-oxo-azepan-3-yl]-carbamic acid tert-butyl ester (0.32 g, 0.83 mmol) in CH2Cl2 (4 mL) is added TFA (1 mL) at room temperature. After 1 h, the reaction is evaporated under vacuum, toluene (20 mL) is added and evaporated under vacuum to remove remaining TFA. The residue is dissolved in CH2Cl2 (20 mL) saturated with NH3 adsorbed on silica and chromatographed (50% EtOAc/CH2Cl2/NH3 then 10% CH3OH/CH2Cl2/NH3) to give 0.207 g (88%) of (3S,6R)-3-amino-6-(6-azido-hexyloxy)-1-methyl-azepan-2-one as an oil. MS (ESI) 284.2 (M+H)+

1. customthe reaction is evaporated under vacuum, toluene (20 mL)
2. additionis added
3. customevaporated under vacuum
4. customto remove
5. dissolutionThe residue is dissolved in CH2Cl2 (20 mL) saturated with NH3
6. customchromatographed (50% EtOAc/CH2Cl2/NH3