反应详情

温度

-10 °C

4.97 g (15 mmol) of 4-[N-(2,4,6-trifluorophenyl)sulfamoyl]-benzoic acid is dissolved in 50 ml of dry dimethylformamide under argon atmosphere, 2.03 g (15 mmol) of hydroxybenzotriazole and 2.42 g (15 mmol) of 2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-ethylamine are added and the solution is cooled to -10° C. At this temperature, 3.09 g (15 mmol) of dicyclohexylcarbodiimide is added to the solution. Then it is stirred for 1 hour at -10° C. and 10 hours at room temperature. The turbid reaction solution is filtered and the filtrate is concentrated by evaporation in a vacuum. The residue is dissolved in 100 ml of ethyl acetate, the solution is shaken out five times with saturated sodium bicarbonate solution and twice with water, the organic phase is dried on sodium sulfate, filtered and concentrated by evaporation. 3.46 g (7.29 mmol)=48.6% of the theoretical yield is obtained as a solid.

1. customThe turbid reaction solution
2. filtrationis filtered
3. concentrationthe filtrate is concentrated by evaporation in a vacuum
4. dissolutionThe residue is dissolved in 100 ml of ethyl acetate
5. stirringthe solution is shaken out five times with saturated sodium bicarbonate solution
6. dry with materialtwice with water, the organic phase is dried on sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated by evaporation
9. custom3.46 g (7.29 mmol)=48.6% of the theoretical yield
10. customis obtained as a solid