HRID625905

反应详情

EQUATION

反应方程式

HRID 625905 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A suspension of 1.007 g (2 mmol) of (R,R)-arformoterol tartrate Form A and 65 mL of methanol was heated to the reflux temperature of the solvent for 30 min. Then, the solution obtained was cooled to 50° C. in 30 min, followed by addition of 90 mL of acetonitrile at the same temperature for 10 minutes. Afterwards, the solution was cooled to 30° C. in 30 minutes and stirred at room temperature for 2 hours. 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 40° C. for 17 hours to provide acetonitrile solvate of (R,R)-Formoterol-L-tartrate, which contained about 2.7% (w/w) of acetonitrile, as determined by TGA analysis.

WORKUP

后处理

  1. temperaturewas heated to the reflux temperature of the solvent for 30 min
  2. customThen, the solution obtained
  3. temperatureAfterwards, the solution was cooled to 30° C. in 30 minutes
  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 40° C. for 17 hours