HRID1364238

反应详情

EQUATION

反应方程式

HRID 1364238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-{[1-(4-{3-[(2R)-2-methylpyrrolidin-1-yl]propoxy}phenyl)-1H-pyrazol-4-yl]carbonyl}morpholine obtained in Example 6-(2) (1.0 g) in ethanol (5 mL), a solution of hydrobromic acid in ethanol (1.5 M, 2.0 mL) was added and stirred at room temperature for 3 hours. The reaction mixture was concentrated under reduced pressure, followed by addition of an ethanol:methanol solution (95:5, 10 mL) to give a solution. This solution was stirred for 3 hours while cooling in an ice bath. The precipitated solid was collected by filtration and dried to give the titled compound (1.1 g) as a colorless powder.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionfollowed by addition of an ethanol
  3. custommethanol solution (95:5, 10 mL) to give a solution
  4. stirringThis solution was stirred for 3 hours
  5. temperaturewhile cooling in an ice bath
  6. filtrationThe precipitated solid was collected by filtration
  7. customdried