反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 55 °C
PROCEDURE
实验过程
A suspension of 407.3 mg (0.82 mmol) of (R,R)-arformoterol tartrate Form B and 15 mL of methanol was heated to the reflux temperature of the solvent for 15 min. Then, the solution obtained was allowed to cool to about 50-60° C., followed by addition of 45 mL of acetonitrile at the same temperature. Afterwards, the solution was cooled to room temperature and stirred for 30 minutes. The product was collected by filtration, washed with acetonitrile and dried under vacuum (2-3 mbar, equivalent to 1.5-2.25 mm Hg) at 60° C. for 2 hours to provide 345.5 mg (85% yield) of acetonitrile solvate of (R,R)-Formoterol-L-tartrate, which contained about 1.6% (w/w) of acetonitrile, as determined by TGA analysis.
WORKUP
后处理
- temperaturewas heated to the reflux temperature of the solvent for 15 min
- customThen, the solution obtained
- temperatureAfterwards, the solution was cooled to room temperature
- filtrationThe product was collected by filtration
- washwashed with acetonitrile
- customdried under vacuum (2-3 mbar, equivalent to 1.5-2.25 mm Hg) at 60° C. for 2 hours