反应详情

TFA (400 mL) was added portionwise to a solution of tert-butyl 4-(5-(5-amino-6-(5-tert-butyl-1,3,4-oxadiazol-2-yl)pyrazin-2-yl)-1-ethyl-1H-1,2,4-triazol-3-yl)piperidine-1-carboxylate (126 g, 253.22 mmol) in DCM (400 mL). The mixture was stirred for 16 hours at room temperature. The mixture was concentrated under reduced pressure, dissolved in DCM (1 L) and added slowly to a vigorously stirred solution of concentrated aqueous ammonia (500 mL) in water at 0° C. The organic solution was separated from the aqueous and concentrated under reduced pressure* to afford 3-(5-tert-butyl-1,3,4-oxadiazol-2-yl)-5-(1-ethyl-3-(piperidin-4-yl)-1H-1,2,4-triazol-5-yl)pyrazin-2-amine (101 g, 100%) as a yellow solid: 1H NMR Spectrum: (DMSO-d6) 1.4-1.52 (12H, m), 1.57-1.73 (2H, m), 1.83-1.93 (2H, m), 2.57-2.7 (2H, m), 2.71-2.84 (1H, m), 2.96-3.09 (2H, m), 4.58 (2H, q), 8.06 (2H, s), 8.84 (1H, s); Mass Spectrum [M+H]+=398.

1. concentrationThe mixture was concentrated under reduced pressure
2. dissolutiondissolved in DCM (1 L)
3. additionadded slowly to a vigorously stirred solution of concentrated aqueous ammonia (500 mL) in water at 0° C
4. customThe organic solution was separated from the aqueous and
5. concentrationconcentrated under reduced pressure*