反应详情

In 10 mL of pyridine, 463 mg (0.957 mmol) of 1-[4-(6-amino-purin-9-yl)phenyl]-3-(4-chloro-3-(trifluoromethyl)phenyl)urea hydrochloride was dissolved, and 455 mg (3.83 mmol) of dimethylformamide dimethylacetal was added thereto and the mixture solution was stirred at room temperature for 16 hours. The reaction solution was concentrated under reduced pressure, and then the residue was triturated with ethyl acetate and collected by filtration, and vacuum dried. The white solid was dissolved in 10 mL of methanol and 4N hydrochloric acid and concentrated under reduced pressure. The residue was triturated with ethyl acetate, collected by filtration, and then vacuum dried to obtain 580 mg (quantitative) of N′-(9-{4-[3-(4-chloro-3-(trifluoromethyl)phenyl)ureido]phenyl}-9H-purin-6-yl)-N,N-dimethylformamidine hydrochloride (Table 1, Compound No. 95) as a white solid.

1. concentrationThe reaction solution was concentrated under reduced pressure
2. customthe residue was triturated with ethyl acetate
3. filtrationcollected by filtration, and vacuum
4. customdried
5. dissolutionThe white solid was dissolved in 10 mL of methanol
6. concentration4N hydrochloric acid and concentrated under reduced pressure
7. customThe residue was triturated with ethyl acetate
8. filtrationcollected by filtration
9. customvacuum dried