反应详情

温度

100 °C

To a suspension of 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 (80 mg, 0.173 mmol) in acetonitrile (1.5 mL) and water (0.4 mL) was added calcium carbonate (51.9 mg, 0.518 mmol) and mercury(II) chloride (141 mg, 0.518 mmol). The mixture was stirred at 80° C. for 5 h and at 100° C. for 6 h. The crude reaction was diluted with EtOAc (150 mL) and washed with aqueous solution of ammonium acetate. The organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo to afford 2-(4-(4-chloro-1H-imidazol-1-yl)-3-methoxyphenylamino)-7,8-dihydro-5H-[1,2,4]triazolo[1,5-a]azepin-9(6H)-one (28 mg, 0.075 mmol, 44% yield). LC-MS (M+H)+ =373.1. The crude product was used in the next step without purification.

1. customThe crude reaction
2. washwashed with aqueous solution of ammonium acetate
3. dry with materialThe organic layer was dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo