反应详情

温度

61.5 °C

A 500 ml reaction vessel equipped with a magnetic stirrer and a reflux condenser was charged with Temozolomide hydrochloride (11.7 grams, 0.0507 mol), acetonitrile (79 ml), acetic acid (2.5 ml) and water (96.5 ml). The reaction mixture was heated to 60-63° C. and stirring was maintained at this temperature for about 10 minutes. The reaction mixture was filtered at this temperature and then cooled to 5° C. for about half an hour to enable crystallization. The crystals thus obtained were collected and washed with water (2×20 ml) and cold acetone (20 ml). The crystals were dried at 40° C. in vacuum to obtain 8.54 grams (0.044 mol) of free Temozolomide base (86.7% yield). Purity (by HPLC): 99.96%.

1. customA 500 ml reaction vessel
2. customequipped with a magnetic stirrer and a reflux condenser
3. temperaturewas maintained at this temperature for about 10 minutes
4. filtrationThe reaction mixture was filtered at this temperature
5. temperaturecooled to 5° C. for about half an hour
6. customcrystallization
7. customThe crystals thus obtained
8. customwere collected
9. washwashed with water (2×20 ml) and cold acetone (20 ml)
10. customThe crystals were dried at 40° C. in vacuum