Reaktionsgleichung
[CH3:1][C:2]([NH:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:6]=1[Cl:12])=[O:3].[N+:13]([O-])([OH:15])=[O:14]>>[CH3:1][C:2]([NH:4][C:5]1[C:10]([N+:13]([O-:15])=[O:14])=[CH:9][CH:8]=[C:7]([Cl:11])[C:6]=1[Cl:12])=[O:3]Komponenten
3
Versuchsvorschrift
Nitric acid (30 ml) is cooled to -5°, and N-methylcarbonyl 2,3-dichloroaniline (9.8 g, 48 mmol) is added to the acid in small portions, with the temperature maintained at -5° or lower. After the addition is complete, the reaction is stirred for 1 hour at +5°. The reaction is then added dropwise to about 150 g of ice-water mixture. The resulting solid is collected by filtration and purified by prep. TLC (developing with 30% ethyl acetate/hexane). The least polar component is isolated to give N-methylcarbonyl 2,3-dichloro-6-nitroaniline.
Aufarbeitung
- temperaturemaintained at -5°
- additionAfter the addition
- filtrationThe resulting solid is collected by filtration
- custompurified by prep
- customThe least polar component is isolated
Quellen und Nachweise
- ORD-Eintrag
- ord-a161289efb534d679a20b921d5c5cdd2
- Quelldatensatz
- uspto-grants-1985_10
- Patentnummer
- US04544400
Verknüpfte Notizen
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