反应详情

温度

35 °C

In a suitable vessel were charged 7-Ethyl-10-hydroxycamptothecin (20 g), methylene dichloride, acetamide (3 gm) and pyridine (60 ml) under nitrogen atmosphere. A solution of [1,4′]bipiperidinyl-1′-carbonyl chloride (17.6 g), methylene dichloride and triethylamine (20 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. The crystalline compound was filtered, washed with hexane and dried under reduced pressure at 50° C. The yield was 28.4 g (95%). HPLC Purity—99.9%

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
6. filtrationThe crystalline compound was filtered
7. washwashed with hexane
8. customdried under reduced pressure at 50° C