Iodoethane → 1,2-Difluoro-4-ethylsulfonylbenzene
Reaktionsgleichung
[F:1][C:2]1[CH:3]=[C:4]([S:9]([OH:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8].[CH2:12](N(CC)CC)[CH3:13].ICC>CN(C=O)C>[CH2:12]([S:9]([C:4]1[CH:5]=[CH:6][C:7]([F:8])=[C:2]([F:1])[CH:3]=1)(=[O:11])=[O:10])[CH3:13]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 90 °C
Versuchsvorschrift
To 3.0 mmol 3,4-difluoro-benzenesulfinic acid and 3.0 mmol triethylamine in 10 ml DMF was added 7.5 mmol iodoethane and the mixture heated at 90° C. for 9 h. The reaction mixture was then poured onto water and extracted three times with ethyl acetate. The combined organic phases were then washed twice with saturated aq. NaCl solution, dried over Na2SO4, and concentrated in vacuo. The residue was chromatographed on silica gel (eluant: ethyl acetate/heptane 1:7) to afford the title compound. MS (m/e): 206.9 (M+H+, 100%)
Aufarbeitung
- additionThe reaction mixture was then poured onto water
- extractionextracted three times with ethyl acetate
- washThe combined organic phases were then washed twice with saturated aq. NaCl solution
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
- customThe residue was chromatographed on silica gel (eluant: ethyl acetate/heptane 1:7)
Quellen und Nachweise
- ORD-Eintrag
- ord-2afca82b88f642d08ee2f4aefd96df3a
- Quelldatensatz
- uspto-grants-2009_10
- Patentnummer
- US07605163B2
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