Sodium hydride → N-[5-(o-chloro-p-trifluoromethyl-phenoxy)-2-nitrobenzoyl]-S,S-dimethyl-sulphoximine
Reaktionsgleichung
[H-].[Na+].[Cl:3][C:4]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:6][C:5]=1[OH:14].F[C:16]1[CH:17]=[CH:18][C:19]([N+:29]([O-:31])=[O:30])=[C:20]([CH:28]=1)[C:21]([N:23]=[S:24]([CH3:27])([CH3:26])=[O:25])=[O:22]>CN(C)C=O>[Cl:3][C:4]1[CH:9]=[C:8]([C:10]([F:12])([F:13])[F:11])[CH:7]=[CH:6][C:5]=1[O:14][C:16]1[CH:17]=[CH:18][C:19]([N+:29]([O-:31])=[O:30])=[C:20]([CH:28]=1)[C:21]([N:23]=[S:24]([CH3:27])([CH3:26])=[O:25])=[O:22]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
0.48 g of sodium hydride is placed in 10 ml of absolute dimethylformamide. 1.96 g of o-chloro-p-trifluoromethyl-phenol are added dropwise and the mixture is stirred for 1 hour. 2.6 g of N-(5-fluoro-2-nitrobenzoyl)-S,S-dimethyl-sulphoximine are added and the mixture is heated to 100° C. for 90 minutes. The mixture is then cooled, poured on to 100 ml of ice-water and extracted with 50 ml of ethyl acetate. The ethyl acetate phase is washed with water, dried and evaporated, and the residue is purified by chromatography and crystallized from diethyl ether. There is obtained 1 g of N-[5-(o-chloro-p-trifluoromethyl-phenoxy)-2-nitrobenzoyl]-S,S-dimethyl-sulphoximine, m.p. 122° C.
Aufarbeitung
- temperatureThe mixture is then cooled
- extractionextracted with 50 ml of ethyl acetate
- washThe ethyl acetate phase is washed with water
- customdried
- customevaporated
- customthe residue is purified by chromatography
- customcrystallized from diethyl ether
Quellen und Nachweise
- ORD-Eintrag
- ord-5a568fe3b2a34f06928bcc3060d41167
- Quelldatensatz
- uspto-grants-1985_12
- Patentnummer
- US04556413
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