Reaktionsgleichung
C[O:2][C:3](=[O:20])[CH2:4][S:5](=[O:19])(=[O:18])[NH:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][C:8]=1[C:14]([F:17])([F:16])[F:15].[OH-].[Na+].Cl.CCOCC.CCCCCC>O1CCOCC1>[F:13][C:10]1[CH:11]=[CH:12][C:7]([NH:6][S:5]([CH2:4][C:3]([OH:20])=[O:2])(=[O:19])=[O:18])=[C:8]([C:14]([F:17])([F:15])[F:16])[CH:9]=1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
2.2 g (6.98 mmol) of 2-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]-acetic acid methyl ester is dissolved in 20 ml of dioxane, and the solution is mixed with 10 ml (20 mmol) of 2N sodium hydroxide solution. A slight warming occurs and the saponification is complete after 10 minutes. The solution is neutralized with 2N hydrochloric acid with pH control and gently evaporated to dryness in a vacuum. The residue is extracted with 30 ml ethyl acetate, the solution is shaken out once with 10 ml of water, the organic phase is dried on magnesium sulfate, filtered and evaporated to dryness. 1.96 g (6.51 mmol)=93.2% of the theoretical yield is obtained. Melting point 120-121° C. (ether/hexane).
Aufarbeitung
- temperatureA slight warming
- customgently evaporated to dryness in a vacuum
- extractionThe residue is extracted with 30 ml ethyl acetate
- customthe organic phase is dried on magnesium sulfate
- filtrationfiltered
- customevaporated to dryness
- custom1.96 g (6.51 mmol)=93.2% of the theoretical yield
- customis obtained
Quellen und Nachweise
- ORD-Eintrag
- ord-6d86645e0c254556a7447a41adb5575d
- Quelldatensatz
- uspto-grants-1992_07
- Patentnummer
- US05130119
Verknüpfte Notizen
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