反应详情

To a solution of 6,6-bis(hydroxymethyl)-6,7,8,9-tetrahydrobenzocyclohepten-5-one (500 mg, 2.27 mmol) in 28 ml of tetrahydrofuran were added, at room temperature, triethylamine (0.35 ml, 2.50 mmol) and 2,4-difluorophenyl isothiocyanate (740 μl, 5.68 mmol). The mixture was heated to reflux for 72 hours, concentrated and purified by column chromatography on silica gel (eluent: 1:2 tert-butyl methyl ether/cyclohexane). The product was obtained in a yield of 234 mg (26%).

1. temperatureThe mixture was heated
2. temperatureto reflux for 72 hours
3. concentrationconcentrated
4. custompurified by column chromatography on silica gel (eluent: 1:2 tert-butyl methyl ether/cyclohexane)
5. customThe product was obtained in a yield of 234 mg (26%)