反应详情

温度

55 °C

A suspension of 348.8 mg (0.70 mmol) of (R,R)-arformoterol tartrate Form B in 15 mL of methanol was heated to the reflux temperature of the solvent for 15 minutes or until a clear yellow solution was obtained. Afterwards, it was cooled to about 60-50° C. and followed by addition of 5 mL aliquots of acetonitrile (total of 45 mL) at the same temperature until a suspension was obtained. The suspension was further cooled to 10-40° C. and stirred at this temperature for 10 minutes. The product was collected by filtration, washed with acetonitrile and dried under vacuum (2 mbar, equivalent to 1.5 mm Hg) at 40° C. for 12 hours to provide 262.4 mg (75% yield) of acetonitrile solvate of (R,R)-Formoterol-L-tartrate, which contained acetonitrile in a range between 2 and 4% (w/w), as determined by 1H-NMR or TGA analysis.

1. temperaturewas heated to the reflux temperature of the solvent for 15 minutes or until a clear yellow solution
2. customwas obtained
3. customwas obtained
4. temperatureThe suspension was further cooled to 10-40° C.
5. filtrationThe product was collected by filtration
6. washwashed with acetonitrile
7. customdried under vacuum (2 mbar, equivalent to 1.5 mm Hg) at 40° C. for 12 hours