反应详情

温度

72 °C

To a solution of N-(4-(4-chloro-1H-imidazol-1-yl)-3-methoxyphenyl)-5-(2-(4-chlorobutyl)-1,3-dithian-2-yl)-1H-1,2,4-triazol-3-amine (110 mg, 0.220 mmol) in DMF (3 mL) was added potassium carbonate (122 mg, 0.881 mmol) and potassium iodide (73.1 mg, 0.440 mmol). The mixture was stirred at 72° C. for 5 h. The mixture was concentrated in vacuo. The residue was purified using silica gel column chromatography (0-80% EtOAc/hexanes, linear gradient) to afford N-(4-(4-chloro-1H-imidazol-1-yl)-3-methoxyphenyl)-5,6,7,8-tetrahydrospiro[[1,2,4]triazolo[1,5-a]azepine-9,2′-[1,3]dithian]-2-amine (90 mg, 0.185 mmol, 84% yield). LC-MS (M+H)+=463.1.

1. concentrationThe mixture was concentrated in vacuo
2. customThe residue was purified