反应详情

To a 16 L reactor was charged amorphous irinotecan acetate (234 g) and ethanol (1300 g). The reaction mixture was heated to reflux. 9N Hydrochloric acid (14.3 wt %, about 89 g) was added until the pH value of the solution was less than 4 in order to dissolve the solid particles. Ethyl acetate (2040 g) was added slowly to the mixture. The mixture was cooled to 0˜10° C. and stirred at this temperature for 1 hour. The solid particles were filtered and washed with cooled ethyl acetate (420 g). The wet cake was dried in vacuum to give 160 g of irinotecan hydrochloride trihydrate form IV.

1. temperatureThe reaction mixture was heated to reflux
2. dissolutionto dissolve the solid particles
3. temperatureThe mixture was cooled to 0˜10° C.
4. filtrationThe solid particles were filtered
5. washwashed with cooled ethyl acetate (420 g)
6. customThe wet cake was dried in vacuum