Water → HCID 58204153, compound

Participants

Reaction Steps

To a mixture of 2-[2-(2,4-Difluoro-phenyl)-2H-[1,2,4]triazol-3-yl]-9-((3R,5S)-3,5-dimethyl-piperazin-1-yl)-4,5-dihydro-6-oxa-1-thia-10-aza-benzo[e]azulene (100 mg, 0.2 mmol), Cesium carbonate (131 mg, 0.4 mmol) in N,N-dimethylformamide (5 mL) was added CH3I (0.025 mL, 0.4 mmol) at −15° C. The mixture was slowly warmed to room temperature and stirred for about 30 min. The reaction mixture was added 30 mL of water. The solid was collected to give 70 mg of 313. Yield=60%. 1H NMR (CDCl3, 400 MHz): δ8.02 (s, 1 H), 7.51-7.46 (m, 1H), 7.11-6.97 (m, 4 H), 6.46 (d, J=8.8 Hz, 1 H), 4.18 (t, J=4.8 Hz, 2 H), 3.85 (d, J=13.6 Hz, 2 H), 3.08 (t, J=4.8 Hz, 2H), 2.59 (t, J=7.2 Hz, 2 H), 2.26-2.19 (m, 4 H), 1.14 (d, J=6.8 Hz, 6 H). ESI-MS: m/z=509 [M+H+]

Provenance & Evidence