反应详情

温度

53 °C

To a solution of 6-amino-2-butoxy-9-{3-[(3-morpholin-4-ylpropyl)amino]propyl}-7,9-dihydro-8H-purine-8-one trihydrochloride (15.00 g, 29.02 mmol) in 10% brine (105.00 g) was added an aqueous 10% sodium carbonate to be neutralized. After adding chloroform (335.7 g), the mixture was heated to 53° C., and the aqueous layer was separated and removed. After an organic layer was concentrated, to the residue was added methanol (296.63 g) and the mixture was raised to 50° C. After methanol (59.33 g) containing maleic acid (6.74 g, 58.04 mmol) was dropped, a white crystal was confirmed. After stirring at 70° C. for 1 hour, the mixture was cooled to 5° C., a crystal was filtered, washed and dried to give the subject compound (17.60 g, 94.8%). Purity: 99.62% (HPLC)

1. customthe aqueous layer was separated
2. customremoved
3. concentrationAfter an organic layer was concentrated, to the residue
4. additionwas added methanol (296.63 g)
5. temperaturethe mixture was raised to 50° C
6. additionwas dropped
7. temperaturethe mixture was cooled to 5° C.
8. filtrationa crystal was filtered
9. washwashed
10. customdried