反应详情

The product of step D (0.132 g, 0.24 mmol) was suspended in 2.0 mL of methanol and the flask was placed in a sonicator bath until the contents were completely dissolved. Next, 95 μL of a 5.0 N solution of sodium hydroxide were added and the reaction was stirred at room temperature overnight. The reaction mixture was then adjusted to pH=5-6 with dropwise addition of 6 N hydrochloric acid, and then concentrated in vacuo. The residue was redissolved in methanol, filtered, and evaporated. The mixture was then 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 0.038 g (35%) of the title compound.

1. customthe flask was placed in a sonicator bath until the contents
2. dissolutionwere completely dissolved
3. concentrationconcentrated in vacuo
4. dissolutionThe residue was redissolved in methanol
5. filtrationfiltered
6. customevaporated
7. customThe mixture was then purified on a silica gel flash chromatography column
8. washeluted with CHCl3 -MeOH-NH4OH (80:15:1)
9. customEvaporation of the purified fractions
10. customdrying in vacuo