Chloroform → Methyl 4-amino-3,5-dichlorobenzoate
Reaktionsgleichung
[NH2:1][C:2]1C=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.S(Cl)([Cl:15])(=O)=O.[OH-].[Na+].[CH:19]([Cl:22])(Cl)Cl>>[NH2:1][C:2]1[C:3]([Cl:15])=[CH:4][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:10][C:19]=1[Cl:22]Komponenten
5
Versuchsvorschrift
Methyl 4-aminobenzoate (25 g.) in dry chloroform (250 ml.) was treated dropwise with sulphuryl chloride (10 ml.) and the mixture heated at reflux for 4 hours. A further supply of sulphuryl chloride (10 ml.) was added and heating continued for a further 2 hours. The reaction mixture was poured onto ice and 2N sodium hydroxide solution was added. The organic solution was separated and the aqueous phase extracted with ethyl acetate. The combined organic solution was dried (anhydrous magnesium sulphate) and evaporated to give methyl 4-amino-3,5-dichlorobenzoate as a solid.
Aufarbeitung
- temperaturethe mixture heated
- temperatureat reflux for 4 hours
- temperatureheating
- additionwas added
- customThe organic solution was separated
- extractionthe aqueous phase extracted with ethyl acetate
- dry with materialThe combined organic solution was dried (anhydrous magnesium sulphate)
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-d5b8192b3b144b0399836676248d826a
- Quelldatensatz
- uspto-grants-1996_03
- Patentnummer
- US05502073
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