Methanesulfonic Acid → HCID 86649776, compound

Participants

Reaction Steps

A suspension of 4-[2-(difluoromethyl)-4-methoxy-1H-benzimidazol-1-yl]-6-(4-morpholinyl)-N-(3-pyridinyl)-1,3,5-triazin-2-amine in MeOH was treated with a slight excess of methanesulfonic acid, to give a clear solution. Addition of EtOAc gave a precipitate, which was collected by filtration and washed with EtOAc. Recrystallization from MeOH/EtOAc gave 4-[2-(difluoromethyl)-4-methoxy-1H-benzimidazol-1-yl]-6-(4-morpholinyl)-N-(3-pyridinyl)-1,3,5-triazin-2-amine methanesulfonate: mp 279-282° C.; 1H NMR (d6-DMSO) δ 10.63 (s, exchangeable with D2O, 1H), 9.19 (s, 1H), 8.55 (d, J=5.5 Hz, 1H), 8.53 (m, 1H), 8.08 (m, 1H), 7.90 (dd, J=8.5, 5.4 Hz, 1H), 7.82 (br t, JHF=53.0 Hz, 1H), 7.43 (t, J=8.2 Hz, 1H), 6.98 (d, J=7.8 Hz, 1H), 4.56 (br m, exchangeable with D20, 1H), 3.99 (s, 3H), 3.86 (m, 4H), 3.75 (m, 4H); Anal. Calcd. for C22H24F2N8O5S: C, 48.0; H, 4.4; N, 20.4. Found: C, 47.8; H, 4.4; N, 20.2%.

Provenance & Evidence