反应详情

To a stirred solution of 1-(4-aminophenyl)-1,2,4-triazole (1.0 g, 6.25 mmol) in MeOH (10 mL) and water (10 mL) was added CaCO3 (1.2 g, 12.0 mmol), followed by a solution of iodine monochloride (1.2 g, 7.38 mmol) in MeOH (10 mL). The reaction mixture was stirred at r.t. for 1.5 h, and then partitioned between EtOAc (100 mL) and aqueous sat. Na2S2O3 (100 mL). The organic fraction was separated, washed with aqueous sat. Na2S2O3 (100 mL), then water (100 mL), brine (50 mL), dried (Na2SO4), filtered and concentrated in vacuo. Purification by column chromatography (SiO2, 0-100% EtOAc/hexanes) gave the title compound (1.2 g, 67%). LCMS (ES+) 286.9 (M+H)+, RT 2.78 minutes (Method 4).

1. custompartitioned between EtOAc (100 mL) and aqueous sat. Na2S2O3 (100 mL)
2. customThe organic fraction was separated
3. washwashed with aqueous sat. Na2S2O3 (100 mL)
4. dry with materialwater (100 mL), brine (50 mL), dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurification by column chromatography (SiO2, 0-100% EtOAc/hexanes)