HRID625904

反应详情

EQUATION

反应方程式

HRID 625904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas heated to the reflux temperature of the solvent for 15 min
  2. customThen, the solution obtained
  3. temperatureAfterwards, the solution was cooled to room temperature
  4. filtrationThe product was collected by filtration
  5. washwashed with acetonitrile
  6. customdried under vacuum (2-3 mbar, equivalent to 1.5-2.25 mm Hg) at 60° C. for 2 hours