反应详情

To a round bottom flask equipped with a magnetic stir bar was added 4-(4-chloro-[1,2,5]thiadiazol-3-yl)-piperazine (7.8 g, 32.6 mmol, 1.0 eq.), dry CH2Cl2 (130 mL), triethyl amine (11.66 g, 16 mL, 115.2 mmol, 3.5 eq). To this mixture cooled in an ice bath was added 1-isocyanato-3,5-bis-trifluoromethyl-benzene (11.6 g, 7.9 ml, 45 mmol, 1.4 eq.) dissolved in dry CH2Cl2 (20 mL) dropwise. The resulting mixture was allowed to warm up to room temperature with stirring. After stirring for 3 hour, the reaction mixture was diluted with EtOAc. This solution was then washed with aqNaHCO3, and brine. The organic layer was dried with Na2SO4, concentrated. The residue was purified by column chromatography using acetate/hexane (1:1 to 3:1), affording 4-(4-Chloro-[1,2,5]thiadiazol-3-yl)-piperazine-1-carboxylic acid (3,5-bis-trifluoromethyl-phenyl)-amide (11.8 g, 79% yield) as a solid.

1. customTo a round bottom flask equipped with a magnetic stir bar
2. temperatureTo this mixture cooled in an ice bath
3. stirringAfter stirring for 3 hour
4. washThis solution was then washed with aqNaHCO3, and brine
5. dry with materialThe organic layer was dried with Na2SO4
6. concentrationconcentrated
7. customThe residue was purified by column chromatography