HRID625903
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 135 mg (0.27 mmol) of (R,R)-arformoterol tartrate Form A and 7.5 mL of methanol was heated to the reflux temperature of the solvent for 10 min. Then, the solution obtained was allowed to cool to about 50-60° C., followed by addition of 19 mL of acetonitrile at the same temperature. Afterwards, the solution was cooled to room temperature and stirred for 1 hour. 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 25° C. for 1 hour to provide acetonitrile solvate of (R,R)-Formoterol-L-tartrate, which contained about 2.5% (w/w) of acetonitrile, as determined by 1H-NMR analysis.
WORKUP
后处理
- temperaturewas heated to the reflux temperature of the solvent for 10 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 25° C. for 1 hour