반응 #741201

반응 방정식

3-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]-benzenesulfonic acid chloride

triethylamine

2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-N-methylethylamine

→

3-[N-(4-Fluoro-2-trifluoromethylphenyl)sulfamoyl]-benzenesulfonic acid-[2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-N-methylethylamide]

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   농축The reaction mixture is then concentrated by evaporation under reduced pressure
2. 2
   추출the residue is extracted with ethyl acetate
3. 3
   기타the extract is chromatographed on silica gel 60 (Merck) with ethyl acetate/hexane
4. 4
   기타9.35 g (16.8 mmol)=84% of the theoretical yield
5. 5
   기타is obtained as an amorphous solid

실험 절차

8.36 g (20 mmol) of 3-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]-benzenesulfonic acid chloride is dissolved in 40 ml of tetrahydrofuran, 2.52 g (25 mmol) of triethylamine and 4.03 (25 mmol) of 2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-N-methylethylamine are added and stirred for 3 hours at 45° C. The reaction mixture is then concentrated by evaporation under reduced pressure, the residue is extracted with ethyl acetate and the extract is chromatographed on silica gel 60 (Merck) with ethyl acetate/hexane. 9.35 g (16.8 mmol)=84% of the theoretical yield is obtained as an amorphous solid.

출처