Reaktionsgleichung
[C:1]([O-:4])(=[O:3])[CH3:2].[C:5]([O-:8])(=[O:7])[CH3:6].[C:9]([O-:12])(=[O:11])[CH3:10].C([O-])(=O)C.[Pb+4:17].[Br:18][C:19]1[CH:20]=[CH:21][C:22]([CH3:28])=[C:23](B(O)O)[CH:24]=1.C(=O)([O-])[O-].[K+].[K+]>>[C:1]([O-:4])(=[O:3])[CH3:2].[C:5]([O-:8])(=[O:7])[CH3:6].[C:9]([O-:12])(=[O:11])[CH3:10].[Br:18][C:19]1[CH:20]=[CH:21][C:22]([CH3:28])=[C:23]([Pb+3:17])[CH:24]=1Komponenten
Reaktionsbedingungen
- Temperatur
- 40 °C
Versuchsvorschrift
To a mixture of lead tetraacetate (11.25 g, 25.40 mmol) and mercuric diacetate (0.40 g, 1.27 mmol), thoroughly flushed with nitrogen, is added anhydrous chloroform (35 ml). This mixture is warmed to 40° C., and 5-bromo-2-methylphenylboronic acid (4.96 g, 23.10 mmol) is added in one portion and the suspension is heated at this temperature for 5 hours. The mixture is then allowed to cool to room temperature, followed by further cooling to 0° C. then powdered anhydrous potassium carbonate (1.61 g) is added with rapid stirring for 5 minutes. The mixture is filtered, the filtrate is concentrated to half its volume, and hexanes added to induce precipitation. This mixture is further concentrated, the solvent decanted, and the solid washed with hexanes to afford 5-bromo-2-methylphenyllead triacetate (10.10 g) as a sandy coloured solid.
Aufarbeitung
- customthoroughly flushed with nitrogen
- additionis added anhydrous chloroform (35 ml)
- temperaturethe suspension is heated at this temperature for 5 hours
- temperatureto cool to room temperature
- temperatureby further cooling to 0° C.
- additionis added
- filtrationThe mixture is filtered
- concentrationthe filtrate is concentrated to half its volume, and hexanes
- additionadded
- customprecipitation
- customthe solvent decanted
- washthe solid washed with hexanes
Quellen und Nachweise
- ORD-Eintrag
- ord-3815df7ca815481aa0e8040fdf2f7242
- Quelldatensatz
- uspto-grants-2014_03
- Patentnummer
- US08680012B2
Verknüpfte Notizen
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