反应详情

A mixture of 113 (1.9 g, 0.005 mol) in THF (200 mL), triethylamine (1.3 mL), and a catalystic amount of 4-dimethylaminopyridine was treated with acetic anhydride (0.9 mL). After stirring over night, the solvent was evaporated and the residue treated with H2O. After 2 h, the mixture was extracted with EtOAc. The extracts were washed with 1 N H2SO4, brine, aqueous NaHCO3, and brine, then the solvent was dried and evaporated to give a floculant white solid (1.94 g) that had the appropriate nmr for the desired material.

1. customthe solvent was evaporated
2. additionthe residue treated with H2O
3. extractionthe mixture was extracted with EtOAc
4. washThe extracts were washed with 1 N H2SO4, brine, aqueous NaHCO3, and brine
5. customthe solvent was dried
6. customevaporated