Water → HCID 18433843, Verbindung
Reaktionsgleichung
[CH2:1]([C:3](=[CH:9][CH3:10])[C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH3:2].[OH-].[Na+].[CH:13]([Cl:16])(Cl)[Cl:14].O>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.ClCCl>[Cl:14][C:13]1([Cl:16])[CH:1]([CH3:2])[C:3]1([CH2:9][CH3:10])[C:4]([O:6][CH2:7][CH3:8])=[O:5]Komponenten
Reaktionsbedingungen
- Temperatur
- 40 °C
Versuchsvorschrift
38 g (0.27 mol) of ethyl 2-ethylbut-2-enoate, 2.2 g (0.01 mol) of benzyltriethylammonium chloride and 57 ml of 50% strength aqueous sodium hydroxide solution were initially charged in 180 ml of dichloromethane. At 35° C. -40° C., 95 ml of chloroform were added dropwise over a period of 1 hour. After a reaction time of 5 hours at 40° C., the mixture was stirred at room temperature for a further 14 hours. For work-up, the reaction solution was poured into 1.5 l of water. The organic phase was removed and the aqueous phase was then extracted with dichloromethane. The combined organic phases were washed with water and, after drying with magnesium sulfate, concentrated. The residue (47 g) was subjected to vacuum distillation. The title compound was isolated as a colorless liquid (25.7 g, 43% yield, boiling point 71° C. at 2 mbar).
Aufarbeitung
- customThe organic phase was removed
- extractionthe aqueous phase was then extracted with dichloromethane
- washThe combined organic phases were washed with water
- dry with materialafter drying with magnesium sulfate
- concentrationconcentrated
- distillationThe residue (47 g) was subjected to vacuum distillation
Quellen und Nachweise
- ORD-Eintrag
- ord-b6638f4efac14d5f9eb8e2599337692d
- Quelldatensatz
- uspto-grants-2002_08
- Patentnummer
- US06441044B1
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