反应详情

温度

35 °C

In a suitable vessel were charged 7-Ethyl-10-hydroxycamptothecin (1 g), methylene dichloride, dimethylformamide (0.186 gm) and pyridine (3 ml) under nitrogen atmosphere. A solution of [1,4′]bipiperidinyl-1′-carbonyl chloride (0.88 g), methylene dichloride and triethylamine (1 ml) was prepared and added to the above suspension and stirred at 30-40° C. for 2 hours. The solvent was distilled out under reduced pressure at 50° C. and hexane was added under stirring as an antisolvent to isolate crystalline compound, which was then filtered, washed with hexane and dried under reduced pressure at 50° C. The yield was 1.30 g (86.89%); HPLC purity—99.8%

1. additionadded to the above suspension
2. distillationThe solvent was distilled out under reduced pressure at 50° C.
3. additionhexane was added
4. stirringunder stirring as an antisolvent
5. customto isolate crystalline compound, which
6. filtrationwas then filtered
7. washwashed with hexane
8. customdried under reduced pressure at 50° C