反应详情

温度

50 °C

Imatinib free base (90 g), methanol (450 mL) and dichloromethane (270 mL) were stirred at 25° C. in round bottom flask in presence of nitrogen. Methanesulfonic acid (18 g) was slowly added to the reaction mixture at 25° C. Water (27 mL) was added and the reaction mixture was stirred for 2 hours. The reaction mixture was heated at 50° C. and concentrated to remove the solvent mixture. The residue was degassed at 60° C. and cooled to 25° C. Methyl tert-butyl ether (630 mL) was added to the reaction mixture and stirred for 45 minutes. The product was filtered and washed with methyl tert-butyl ether. The product was dried at 60° C. under high vacuum for 10 hours to obtain amorphous imatinib mesylate. Water content 0.90%.

1. concentrationconcentrated
2. customto remove the solvent mixture
3. customThe residue was degassed at 60° C.
4. temperaturecooled to 25° C
5. additionMethyl tert-butyl ether (630 mL) was added to the reaction mixture
6. stirringstirred for 45 minutes
7. filtrationThe product was filtered
8. washwashed with methyl tert-butyl ether
9. customThe product was dried at 60° C. under high vacuum for 10 hours