反应详情

A free form (502 mg) of (R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one was measured in a reaction test tube, aqueous ethanol (5.8 mL, ethanol:water=8:1) was added and the mixture was completely dissolved by heating under reflux. Thereto was added aqueous phosphoric acid solution (501 μL, solution prepared by diluting commercially available 85% phosphoric acid (2.02 g) with the above-mentioned aqueous ethanol to scale up to 10 mL), and the mixture was stirred at room temperature for one day and left standing. The precipitate was collected by filtration. The precipitate (301 mg) was measured in a reaction test tube, and aqueous ethanol (2.6 mL, ethanol:water=4:1) was added. The mixture was completely dissolved by heating under reflux, stirred at room temperature for one day and left standing. The precipitate was collected by filtration, and dried under reduced pressure at 50° C. for 5 hr to give the title compound (264 mg).

1. dissolutionthe mixture was completely dissolved
2. temperatureby heating
3. temperatureunder reflux
4. customprepared
5. waitleft
6. filtrationThe precipitate was collected by filtration
7. customThe precipitate (301 mg) was measured in a reaction test tube
8. additionaqueous ethanol (2.6 mL, ethanol:water=4:1) was added
9. dissolutionThe mixture was completely dissolved
10. temperatureby heating
11. temperatureunder reflux
12. stirringstirred at room temperature for one day
13. waitleft
14. filtrationThe precipitate was collected by filtration
15. customdried under reduced pressure at 50° C. for 5 hr