反应详情

tert-Butyl 4-(5-(5-amino-6-(5-tert-butyl-1,3,4-oxadiazol-2-yl)pyrazin-2-yl)-1-methyl-1H-1,2,4-triazol-3-yl)piperidine-1-carboxylate (36.81 g, 76.12 mmol) was added to a solution of 2,2,2-trifluoroacetic acid (100 mL, 1305.87 mmol) in DCM (100 mL). The mixture was stirred for 3 hours at room temperature. The mixture was concentrated under reduced pressure. The residue was dissolved in DCM (1.5 L) and added to vigorously stirred concentrated ammonia (150 mL) in water (400 mL). The aqueous was washed with DCM (400 mL) and the combined organic solutions were dried with magnesium sulfate, filtered and concentrated to dryness to afford 3-(5-tert-butyl-1,3,4-oxadiazol-2-yl)-5-(1-methyl-3-(piperidin-4-yl)-1H-1,2,4-triazol-5-yl)pyrazin-2-amine (30.0 g, 103%) as a yellow solid:

1. concentrationThe mixture was concentrated under reduced pressure
2. dissolutionThe residue was dissolved in DCM (1.5 L)
3. additionadded
4. stirringto vigorously stirred concentrated ammonia (150 mL) in water (400 mL)
5. washThe aqueous was washed with DCM (400 mL)
6. dry with materialthe combined organic solutions were dried with magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated to dryness