反应详情

温度

81 °C

5-[4-[2-(N-methyl-N-(2-pyridyl)amino)ethoxy]benzyl]thiazolidine-2,4-dione (rosiglitazone free base, 50 gms, 0.140 mol) was stirred with 250 ml of dry acetonitrile and a suspension of maleic acid (19.50 gms, 0.168 mol) in 100 ml of dry acetonitrile was added at 27° C. to obtain a clear solution, followed by reflux for 30 minutes at 80-82° C. The reaction mass was gradually allowed to cool to 30° C. and stirred for 5 hours at 25-30° C. The precipitated solid was filtered under argon atmosphere and washed with 50 ml of dry acetonitrile. The filtered solid obtained was dried under vacuum at 30° C. for 5 hours, and at 50° C. for 6 hours, to obtain rosiglitazone maleate Form A (45 gms) in 71% yield.

1. additionwas added at 27° C.
2. customto obtain a clear solution
3. temperatureto cool to 30° C.
4. filtrationThe precipitated solid was filtered under argon atmosphere
5. washwashed with 50 ml of dry acetonitrile
6. customThe filtered solid obtained
7. customwas dried under vacuum at 30° C. for 5 hours
8. waitat 50° C. for 6 hours