Reaktionsgleichung
[CH3:1][C:2]([CH3:9])=[CH:3][CH2:4][CH2:5][CH:6]([OH:8])[CH3:7].[C:10](O)(=[O:14])/[CH:11]=[CH:12]/[CH3:13].CC1C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[CH3:7][CH:6]([O:8][C:10](=[O:14])[CH:11]=[CH:12][CH3:13])[CH2:5][CH2:4][CH:3]=[C:2]([CH3:9])[CH3:1]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 121.5 °C
Versuchsvorschrift
6-Methyl-hept-5-en-2-ol (256 g, commercially available at IFF), crotonic acid (193 g), PTSA (2.5 g), and toluene (250 mL) were charged into a 2-L reaction flask fitted with a mechanical stirrer, a thermocouple, a Dean-Stark trap, and a condenser. The reaction mixture was heated to reflux at about 110-133° C. Water was removed azeotropically. The reaction was aged at reflux for about 6 hours until no more water evolved. The reaction mixture was cooled to under 60° C. and quenched with water (300 mL). The aqueous and organic layers were split. The organic layer was subsequently washed with sodium carbonate (2%, 300 mL) and further fractional distilled to provide but-2-enoic acid 1,5-dimethyl-hex-4-enyl ester (204 g) with a boiling point of 98° C. at 4 mmHg.
Aufarbeitung
- customfitted with a mechanical stirrer
- temperatureThe reaction mixture was heated
- customWater was removed azeotropically
- temperatureat reflux for about 6 hours until no more water
- temperatureThe reaction mixture was cooled to under 60° C.
- customquenched with water (300 mL)
- customThe aqueous and organic layers were split
- washThe organic layer was subsequently washed with sodium carbonate (2%, 300 mL)
- distillationfurther fractional distilled
Quellen und Nachweise
- ORD-Eintrag
- ord-c672b3be4f6641ce8464626d717c7fad
- Quelldatensatz
- uspto-grants-2014_07
- Patentnummer
- US08785677B1
Verknüpfte Notizen
Wird geladen…