反应详情

Under an atmosphere of argon protective gas and at room temperature, triethylamine (11.1 mg, 140 mmol, 2.6 eq.) and methanesulfonyl chloride (41 mg, 360 mmol, 10 eq.) were added to a solution of benzyl{(7R)-6-cyano-7-(4-cyanophenyl)-5-methyl-4-[3-(trifluoromethyl)phenyl]-4,7-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-2-yl}carbamate (20 mg, 36 mmol; Example 38) in dry pyridine (2 ml) and THF (2 ml), and the mixture was stirred for 12 h. The reaction mixture was then 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 (17.4 mg, 72% of theory).

1. concentrationThe reaction mixture was then concentrated under reduced pressure
2. customdirectly purified by preparative HPLC (Reprosil C18 column, 30×200 mm; mobile phase: acetonitrile-water-0.1% TFA)
3. customAfter lyophilization, the product was obtained as a solid (17.4 mg, 72% of theory)