反应详情

TFA (0.771 ml) was added to a stirred suspension of tert-butyl 4-[4-[6-amino-5-(1,3-benzoxazol-2-yl)-3-pyridyl]triazol-1-yl]piperidine-1-carboxylate (231 mg) dissolved in dichloromethane (5 ml) at room temperature. The resulting solution was stirred for 2 hours. Excess TFA was removed by azeotropic concentration with toluene. The residue was taken off with dichloromethane-methanol and treated with methanolic ammonia (7 M). The mixture was concentrated to dryness and the resulting solid was triturated with diethyl ether. The resultant solid was collected by filtration, washed with diethyl ether followed by petroleum ether and dried under vacuum at 60° C. to give 3-(1,3-benzoxazol-2-yl)-5-[1-(4-piperidyl)triazol-4-yl]pyridin-2-amine (180 mg) as a solid; NMR Spectrum: (DMSOd6+TFAd) 2.20-2.32 (m, 2H), 2.38-2.48 (m, 2H), 3.7-3.30 (m, 2H), 3.47-3.58 (m, 2H), 4.92-5.02 (m, 1H), 7.54 (ddd, 1H), 7.59 (ddd, 1H), 7.90 (d, 1H), 7.95 (dd, 1H), 8.84 (d, 1H), 8.96 (s, 1H), 9.24 (d, 1H); Mass spectrum: M+H+: 362

1. customExcess TFA was removed by azeotropic concentration with toluene
2. additiontreated with methanolic ammonia (7 M)
3. concentrationThe mixture was concentrated to dryness
4. customthe resulting solid was triturated with diethyl ether
5. filtrationThe resultant solid was collected by filtration
6. washwashed with diethyl ether
7. customdried under vacuum at 60° C.