Reaktionsgleichung
[CH2:1]([O:3][C:4](=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[Br:9]Br>>[C:4](=[O:8])([O:5][CH2:6][CH3:7])[O:3][CH:1]([Br:9])[CH3:2]Komponenten
3
Versuchsvorschrift
585 g Diethylcarbonate (4.92 mole) was heated by an external 1500 w iodine quartz lamp. The mixture was allowed to reflux (temperature 125°) by the heat evolved from the lamp. 318.2 g (2.0 mole) of bromine is added slowly during 3 hours through a dip-pipe at such a rate that the solution colour was yellow to light orange. The temperature dropped to ca. 120° at the beginning of the addition, but rose again slowly. When all the bromine was consumed the temperature was 137°. The reaction mixture was cooled and treated as described in Example 2. Fractional distillation afforded 1-bromoethyl ethyl carbonate in a 68.5% yield. The earlier fraction contained about 6.5% more of 1-bromoethyl ethyl carbonate.
Aufarbeitung
- temperatureto reflux (temperature 125°) by the heat
- additionThe temperature dropped to ca. 120° at the beginning of the addition
- customWhen all the bromine was consumed the temperature
- customwas 137°
- temperatureThe reaction mixture was cooled
- additiontreated
- distillationFractional distillation
Quellen und Nachweise
- ORD-Eintrag
- ord-6b42669822d24a26898cdf30aa43b07e
- Quelldatensatz
- uspto-grants-1989_12
- Patentnummer
- US04889929
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