反应详情

温度

65 °C

To 4-(1-(4-(trifluoromethyl)phenyl)-1H-1,2,4-triazol-3-yl)aniline (0.496 g, 1.63 mmol) in a 25 mL vial equipped with a stir bar, Vigreux column, and nitrogen inlet was added tetrahydrofuran (4.08 mL) followed by 1-isopropyl-2-isothiocyanatobenzene (0.826 ml, 4.89 mmol). The reaction was heated to 65° C. overnight. The reaction was cooled to room temperature. The reaction mixture was diluted with dichloromethane and washed with water. The aqueous layer was extracted with dichloromethane (2×). The organic layers were poured through a phase separator and concentrated. Purification by flash column chromatography using 0-20% ethyl acetate/B, where B=1:1 dichloromethane/hexanes as eluent provided a white solid. The solid was dried at 55° C. at about 25 in. Hg providing the title compound as a white solid (0.361 g, 46%).

1. temperatureThe reaction was cooled to room temperature
2. washwashed with water
3. extractionThe aqueous layer was extracted with dichloromethane (2×)
4. additionThe organic layers were poured through a phase separator
5. concentrationconcentrated
6. customPurification by flash column chromatography
7. customprovided a white solid
8. customThe solid was dried at 55° C. at about 25 in