反应详情

To a solution of 1.518 g (3.66 mmol) of the product of Step A dissolved in 8.0 mL of methanol was added 1.0 mL of a 5.0M solution of aqueous sodium hydroxide. The reaction was stirred at room temperature and monitored by TLC (80:15:1 CHCl3 --MeOH--NH4OH). After 1.5 hours the reaction was judged to be complete and the reaction mixture was adjusted to pH=5 with 1.0N HCl. The reaction mixture was then partitioned between EtOAc and water, separated, dried (MgSO4), filtered, and evaporated. The residue was purified on a silica gel flash chromatography column eluted with CHCl3 --MeOH--NH4OH (80:15:1); evaporation of the purified fractions and drying in vacuo afforded the title compound as an amorphous foam.

1. customThe reaction mixture was then partitioned between EtOAc and water
2. customseparated
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified on a silica gel flash chromatography column
7. washeluted with CHCl3 --MeOH--NH4OH (80:15:1)
8. customevaporation of the purified fractions
9. customdrying in vacuo