反应详情

Under an atmosphere of argon protective gas, (7R)-2-amino-7-(4-cyanophenyl)-5-methyl-4-[3-(trifluoromethyl)phenyl]-4,7-dihydro[1,2,4]triazolo[1,5-a]pyrimidine-6-carbonitrile hydrochloride (22 mg, 48 mmol) was dissolved in abs. pyridine (5 ml). At room temperature, acetic anhydride (98 mg, 960 μmol, 20 eq.) was added. Once analysis of the reaction by TLC showed substantial conversion (a few hours), the reaction mixture was concentrated under reduced pressure and directly purified by preparative HPLC (Reprosil C18 column, 30×200 mm; mobile phase: acetonitrile-water-0.1% TFA). After lyophilization, the product was obtained as a solid (20.6 mg, 93% of theory).

1. customOnce analysis of the reaction by TLC
2. customconversion (a few hours)
3. concentrationthe reaction mixture was concentrated under reduced pressure
4. customdirectly purified by preparative HPLC (Reprosil C18 column, 30×200 mm; mobile phase: acetonitrile-water-0.1% TFA)
5. customAfter lyophilization, the product was obtained as a solid (20.6 mg, 93% of theory)