反应详情

Referring to scheme 27, Compound 99 (1.48 g, 2 mmol) is mixed with succinic anhydride (0.200 g, 2 mmol) and DMAP (0.244 g, 13 mmol) and dried in a vacuum at 40° C. overnight. The mixture is dissolved in anhydrous dichloromethane (5 mL), triethylamine (0.606 g, 0.96 mL, 6 mmol) is added and the solution stirred at room temperature under argon atmosphere for 16 h. It is then diluted with dichloromethane (100 mL) and washed with ice cold aqueous citric acid (5% wt., 100 mL) and water (2×100 mL) The organic phase is dried over anhydrous sodium sulfate and concentrated to dryness. The crude product is purified by column chromatography to afford compound 101.

1. customdried in a vacuum at 40° C. overnight
2. dissolutionThe mixture is dissolved in anhydrous dichloromethane (5 mL)
3. washwashed with ice cold aqueous citric acid (5% wt., 100 mL) and water (2×100 mL) The organic phase
4. dry with materialis dried over anhydrous sodium sulfate
5. concentrationconcentrated to dryness
6. customThe crude product is purified by column chromatography