反应详情

Cyclohexylisocyanate (13 ul, 0.1 mmol; [3173-53-3]) was added at ambient temperature to a solution of cyclohexyl-(2-phenyl-2H-indazol-3-yl)-amine (30 mg, 0.1 mmol) in toluene (0.4 ml) under an argon atmosphere. The solution was heated under reflux conditions for 12 h, cyclohexylisocyanate (7 μl, 60 μmol; [3173-53-3]) was added and heating was continued for further 6 h. The solvent was removed under reduced pressure to give a brown oil which was purified by preparative thin layer chromatography (silica gel, iPrOAc/heptane) to give the title compound (11 mg, 26 μmol; 27%) as off-white solid. MS: m/e=417.4 [M+H+].

1. temperatureThe solution was heated under reflux conditions for 12 h
2. temperatureheating
3. customThe solvent was removed under reduced pressure
4. customto give a brown oil which
5. customwas purified by preparative thin layer chromatography (silica gel, iPrOAc/heptane)