Reaktionsgleichung
O[CH2:2][NH:3][C:4](=[O:9])[C:5]([F:8])([F:7])[F:6].[Cl:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([Cl:17])[C:12]=1[N+:18]([O-:20])=[O:19].OS(O)(=O)=O>>[N+:18]([C:12]1[C:11]([Cl:10])=[C:16]([CH:15]=[CH:14][C:13]=1[Cl:17])[CH2:2][NH:3][C:4](=[O:9])[C:5]([F:8])([F:7])[F:6])([O-:20])=[O:19]Komponenten
4
Reaktionsbedingungen
- Temperatur
- 75 °C
Versuchsvorschrift
N-(Hydroxymethyl)trifluoroacetamide (6.6 mmol; 0.946 g) is added to a mixture of 2,6-dichloro-nitrobenzene (0.899 mL; 6.6 mmol) and conc. H2SO4 (15 mL) at 75° C. The mixture is stirred at 75° C. overnight, poured into ice water and stirred for 1 h. The precipitate is collected by filtration and dried. Yield 0.32 g (15%). MS [M−H]−=315, HPLC-method B: Rt=1.43 min.
Aufarbeitung
- stirringstirred for 1 h
- filtrationThe precipitate is collected by filtration
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-553a012956504cd28fabbf1743ebf0b1
- Quelldatensatz
- uspto-grants-2014_06
- Patentnummer
- US08759537B2
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