反应详情

温度

70 °C

To a suitable vessel were charged amorphous irinotecan acetate (6.35 g) and ethanol (45 mL). The resulting mixture was heated to reflux (about 70° C.) and remained as a suspension. 2N HCl (5.4 mL) was added to the reaction mixture to adjust the pH to less than 4. N-heptane (25 mL) and ethanol (30 mL) were added to the resulting mixture. The solution was then cooled to 0˜10° C. and stirred at this temperature for 1 hour, and then charged with 200 mL of ethyl acetate in order to perform a solvent swap. The solution was then filtrated and washed with ethyl acetate (50 mL). The solid was dried in vacuum. Due to a lower than expected water content, the solid was heated under high humidity for one hour and then cooled to give irinotecan hydrochloride trihydrate Form I (6.6 g).

1. temperatureThe resulting mixture was heated
2. temperatureThe solution was then cooled to 0˜10° C.
3. filtrationThe solution was then filtrated
4. washwashed with ethyl acetate (50 mL)
5. customThe solid was dried in vacuum
6. temperatureDue to a lower than expected water content, the solid was heated under high humidity for one hour
7. temperaturecooled