反应详情

Referring to scheme 19, Compound 77 (2 g, 3 mmol) was mixed with succinic anhydride (0.600 g, 6 mmol) and DMAP (0.366 g, 3 mmol) and dried in a vacuum at 40° C. overnight. The mixture was dissolved in anhydrous dichloromethane (5 mL), triethylamine (0.913 g, 1.25 mL, 9 mmol) was added and the solution was stirred at room temperature under argon atmosphere for 4 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 using 6% MeOH/DCM to afford compound 79 as white solid (2.05 g, 89% yield; Rf=0.4 in 10% MeOH/CHCl3).

1. customdried in a vacuum at 40° C. overnight
2. dissolutionThe mixture was dissolved in anhydrous dichloromethane (5 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