Reaktionsgleichung
Cl.[NH2:2][C:3]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6].[CH3:14]O>>[NH2:2][C:3]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][C:4]=1[C:5]([O:7][CH3:14])=[O:6]Komponenten
4
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
Hydrogen chloride gas was bubbled through a solution of 2-amino-5-methoxybenzoic acid (5.0 g, 30 mmol) in MeOH (200 mL) for 30 minutes. The solution was heated at 60° C. overnight. The reaction was cooled and the solvent removed in vacuo. The residue was dissolved in water, basified with 5M NaOH and extracted twice with ether. The ether extracts were washed with 5M NaOH and water, dried (MgSO4), filtered and concentrated in vacuo to give i-e (4.25 g, 78%): MS m/z=182 (M+H).
Aufarbeitung
- temperatureThe reaction was cooled
- customthe solvent removed in vacuo
- dissolutionThe residue was dissolved in water
- extractionextracted twice with ether
- washThe ether extracts were washed with 5M NaOH and water
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give i-e (4.25 g, 78%)
Quellen und Nachweise
- ORD-Eintrag
- ord-7fc8fb3b35f1478b8069aee2cc738136
- Quelldatensatz
- uspto-grants-2011_05
- Patentnummer
- US07935694B2
Verknüpfte Notizen
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