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:24]=[CH:23][C:22](B(O)O)=[C:21]([CH2:28][CH3:29])[CH:20]=1>>[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:24]=[CH:23][C:22]([Pb+3:17])=[C:21]([CH2:28][CH3:29])[CH:20]=1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 40 °C
Versuchsvorschrift
To a mixture of lead tetraacetate (53 g, 0.12 mol) and mercuric diacetate (2.5 g, 0.0078 mol), thoroughly flushed with nitrogen, is added anhydrous chloroform (250 ml). This mixture is warmed to 40° C. and 4-bromo-2-ethylphenylboronic acid (25 g, 0.11 mol) is added in one portion and the mixture is stirred and heated at this temperature for 4 hours. After cooling to room temperature, cooled in an ice bath, filtered through a plug of diatomaceous earth and the filtrate is concentrated to approximately a quarter of its volume. Hexane is added to induce crystallization and the solvents evaporated under reduced pressure. Trituration with hexane gives 4-bromo-2-ethylphenyl lead triacetate (28 g).
Aufarbeitung
- customthoroughly flushed with nitrogen
- additionis added anhydrous chloroform (250 ml)
- temperatureheated at this temperature for 4 hours
- temperatureAfter cooling to room temperature
- temperaturecooled in an ice bath
- filtrationfiltered through a plug of diatomaceous earth
- concentrationthe filtrate is concentrated to approximately a quarter of its volume
- additionHexane is added
- customcrystallization
- customthe solvents evaporated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-66c96b4989b54d7cac56c093b825e16e
- Quelldatensatz
- uspto-grants-2014_11
- Patentnummer
- US08895761B2
Verknüpfte Notizen
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