反应详情

Referring to scheme 5, Compound 12 (5.6 g, 4.8 mmol) was mixed with succinic anhydride (0.727 g, 7.26 mmol) and DMAP (0.062 g, 0.5 mmol) and dried in a vacuum at 40° C. overnight. The mixture was dissolved in anhydrous dichloromethane (20 mL), triethylamine (1.52 g, 2 mL, 15 mmol) was added and the solution was stirred at room temperature under argon atmosphere for 16 h. It was then diluted with dichloromethane (50 mL) and washed with ice cold aqueous citric acid (5% wt., 50 mL) and water (2×50 mL). The organic phase was dried over anhydrous sodium sulfate and concentrated to dryness. The crude product was purified by column chromatography to afford compound 14 as white solid (2.85 g, 47% yield; Rf=0.65 in 10% MeOH/CHCl3).

1. customdried in a vacuum at 40° C. overnight
2. dissolutionThe mixture was dissolved in anhydrous dichloromethane (20 mL)
3. washwashed with ice cold aqueous citric acid (5% wt., 50 mL) and water (2×50 mL)
4. dry with materialThe organic phase was dried over anhydrous sodium sulfate
5. concentrationconcentrated to dryness
6. customThe crude product was purified by column chromatography