反应详情

3.63 g (10 mmol) of 4-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]-benzoic acid is suspended in 36 ml of ethyl acetate, 2.38 g (20 mmol) of thionylchloride is added and the suspension is heated to boiling temperature. After 15 minutes a clear solution is present, after 1 hour the formation of the acid chloride is complete. The solution is evaporated to dryness under reduced pressure, the residue is concentrated by evaporation in a vacuum twice with 50 ml of dichloromethane each and the dissolved in 36 ml of dioxane. 1.21 g (12 mmol) of triethylamine and 1.93 g (12 mmol) of 2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-ethylamine are added to this solution and it is stirred for 5 hours at room temperature. The reaction solution is then evaporated to dryness in a vacuum, the residue is extracted with ethyl acetate, the ethyl acetate extract is concentrated by evaporation in a vacuum and the residue is chromatographed on silica gel 60 (Merck) with ethyl acetate/hexane. 3.19 g (6.3 mmol) =63% of the theoretical yield of the product is obtained as an amorphous solid.

1. temperaturethe suspension is heated
2. customThe solution is evaporated to dryness under reduced pressure
3. concentrationthe residue is concentrated by evaporation in a vacuum twice with 50 ml of dichloromethane each and the
4. dissolutiondissolved in 36 ml of dioxane
5. customThe reaction solution is then evaporated to dryness in a vacuum
6. extractionthe residue is extracted with ethyl acetate
7. extractionthe ethyl acetate extract
8. concentrationis concentrated by evaporation in a vacuum
9. customthe residue is chromatographed on silica gel 60 (Merck) with ethyl acetate/hexane
10. custom3.19 g (6.3 mmol) =63% of the theoretical yield of the product is obtained as an amorphous solid