反应详情

A solution of trans-{4-[4-amino-5-(4-phenoxy-phenyl)-imidazo[5,1-f][1,2,4]triazin-7-yl]-cyclohexylmethyl}-carbamic acid benzyl ester (20.0 mg, 0.0364 mmol) and 4 M of HCl in 1,4-dioxane (2 mL) was heated to reflux overnight. The solution was concentrated in vacuo and left to dry in the vacuum oven overnight to afford the title compound as a yellow solid. 1H NMR (400 MHz, CDCl3): δ=1.23-1.37 (m, 2H), 1.83-1.99 (m, 3H), 2.03-2.09 (m, 2H), 2.15-2.24 (m, 2H), 2.86 (d, J=4.0 Hz, 2H), 3.44-3.56 (m, 1H), 7.12 (d, J=8.1 Hz, 2H), 7.17-7.26 (m, 3H), 7.44 (t, J=7.8 Hz, 3H), 7.66 (d, J=3.5 Hz, 2H), 8.00-8.10 (m, 1H). MS (ES+): m/z 415.02 (100) [MH+]. HPLC: tR=2.26 min (OpenLynx, polar—5 min).

1. temperatureto reflux overnight
2. concentrationThe solution was concentrated in vacuo
3. waitleft
4. customto dry in the vacuum oven overnight