反应详情

温度

45.29999923706055 °C

0.3 Kg of 10-hydroxy camptothecin (Formula IV) prepared according to Example-1 was suspended in 6 L of acetic acid and stirred for 5 minutes. The obtained solution was charged into a reactor and stirred for 20 minutes. 0.51 L of a 40% aqueous solution of dimethyl amine and 0.078 L of a 37% of aqueous solution of formaldehyde were charged into the reactor, the temperature raised to 45.3° C. and the reaction mixture stirred for 2 hours at 45.3° C. The reaction solution was allowed to cool to 34.8° C. and then cooled to 27.5° C. 42 L of acetone was charged into above reaction solution and stirred for 1 hour at 27.5° C. for complete precipitation. The formed solid was filtered and the reactor rinsed with 1.5 L of acetone. The wet solid was washed with the rinsing and then washed with 0.3 L of 1-propanol. The resultant solid was suction dried for 20 minutes and then dried for 5 hours at 52° C. under a vacuum of 690 mm Hg to afford 330 g of title compound having a purity by HPLC of about 98.9%.

1. additionThe obtained solution was charged into a reactor
2. stirringstirred for 20 minutes
3. stirringthe reaction mixture stirred for 2 hours at 45.3° C
4. temperatureto cool to 34.8° C.
5. temperaturecooled to 27.5° C
6. stirringstirred for 1 hour at 27.5° C. for complete precipitation
7. filtrationThe formed solid was filtered
8. washthe reactor rinsed with 1.5 L of acetone
9. washThe wet solid was washed with the rinsing and
10. washthen washed with 0.3 L of 1-propanol
11. customThe resultant solid was suction dried for 20 minutes
12. customdried for 5 hours at 52° C. under a vacuum of 690 mm Hg