反应详情

A free form (1 g) of (R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one was measured, ethanol (40 ml) was added and the mixture was completely dissolved by heating under reflux. Thereto was added commercially available 85% phosphoric acid (200 μL) and the mixture was left stirring at room temperature for 1 hr. The precipitate was collected by filtration and dissolved again in water (1 mL) at 80° C. Ethanol (8 mL) was added and the mixture was left standing at room temperature for 1 hr. The resulting precipitate was collected by filtration and dried under reduced pressure at 50° C. for 9 hr to give the title compound (838 mg).

1. dissolutionthe mixture was completely dissolved
2. temperatureby heating
3. temperatureunder reflux
4. waitthe mixture was left
5. filtrationThe precipitate was collected by filtration
6. dissolutiondissolved again in water (1 mL) at 80° C
7. additionEthanol (8 mL) was added
8. waitthe mixture was left
9. waitstanding at room temperature for 1 hr
10. filtrationThe resulting precipitate was collected by filtration
11. customdried under reduced pressure at 50° C. for 9 hr