Reaktionsgleichung
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([CH:11]=[C:12]([CH3:15])[CH:13]=[O:14])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH2:16]([O:20][CH:21]=[CH2:22])[CH:17]([CH3:19])[CH3:18]>C1(C=CC(O)=CC=1)O>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([C:11]2[CH2:22][CH:21]([O:20][CH2:16][CH:17]([CH3:19])[CH3:18])[O:14][CH2:13][C:12]=2[CH3:15])=[CH:9][CH:10]=1)([CH3:4])([CH3:2])[CH3:3]Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 220 °C
Versuchsvorschrift
3,000 g of 3-(4-tert.-butylphenyl)-2-methylprop-2-enal III and 2,000 g of vinyl isobutyl ether IV are introduced into a 10 l stirred autoclave, and 5 g of hydroquinone are added to the reaction mixture for stabilization. The autoclave is closed and then flushed with nitrogen, after which it is heated to 220° C., maintained under these conditions for 18 hours and then let down and opened. The reaction mixture (4,855 g) consists of about 39.6% of the desired product V. When the reaction mixture is worked up by fractionation in a laboratory column containing 10 sieve trays, a total of 1,379 g of the compound V of boiling point 135°-146° C. under 2 mbar are obtained from the 1,923 g shown to be present in the crude mixture by gas chromatographic analysis. This corresponds to a yield of 23%, based on the starting material III employed. 1,745 g of III, which contains some product V, are recovered. The last-mentioned amounts are reused for the reaction with vinyl isobutyl ether.
Aufarbeitung
- additionare added to the reaction mixture for stabilization
- customThe autoclave is closed
- customflushed with nitrogen
- temperaturemaintained under these conditions for 18 hours
- additioncontaining 10 sieve trays
Quellen und Nachweise
- ORD-Eintrag
- ord-271966fa3bd34eb7b7b40b0f1c058e96
- Quelldatensatz
- uspto-grants-1993_05
- Patentnummer
- US05212183
Verknüpfte Notizen
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