反应详情

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) (2.62 g) in ethyl acetate (18 mL), a solution of hydrochloric acid in ethyl acetate (4 M, 2.46 mL) was added and stirred at room temperature for 30 minutes. The precipitated crystal was collected by filtration to give a crude crystal (2.9 g). A suspension of the resulting crude crystal in ethanol (9 mL) was heated under reflux to give a solution, which was then filtered. After addition of ethanol (6 mL), the filtrate was stirred for 30 minutes while cooling to room temperature. The mixture was further stirred in an ice bath for 1.5 hours, and the precipitated crystal was collected by filtration and dried to give the titled compound (2.67 g) as a colorless powder.

1. filtrationThe precipitated crystal was collected by filtration
2. customto give a crude crystal (2.9 g)
3. temperaturewas heated
4. temperatureunder reflux
5. customto give a solution, which
6. filtrationwas then filtered
7. additionAfter addition of ethanol (6 mL)
8. stirringthe filtrate was stirred for 30 minutes
9. temperaturewhile cooling to room temperature
10. stirringThe mixture was further stirred in an ice bath for 1.5 hours
11. filtrationthe precipitated crystal was collected by filtration
12. customdried