Reaktionsgleichung
[C:1]([CH:5]1[CH2:10][CH2:9][CH:8]([CH:11]=O)[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[C:13]([C:18](=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH3:19])([O:15][CH2:16][CH3:17])=[O:14].C(O)(=O)C1C=CC=CC=1>C1(C)C=CC=CC=1.CO.O>[CH2:16]([O:15][C:13](=[O:14])[C:18]([CH3:19])=[CH:11][CH:8]1[CH2:7][CH2:6][CH:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[CH2:10][CH2:9]1)[CH3:17]Komponenten
6
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
A mixture of 20.2 g of 4-tert.butyl-cyclohexane-1-carboxaldehyde, 52 g of (α-carbethoxy-ethylidene)-triphenyl-phosphorane and 3.6 g of benzoic acid in 120 ml of toluene is heated at reflux for 16 hours under nitrogen gasification and the toluene is evaported. The oily-crystalline residue is dissolved in 600 ml of methanol/water (4:1) and exhaustively extracted with hexane. The combined hexane extracts are washed with sodium bicarbonate solution and water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 3-(4-tert.butyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester of boiling point 99° C./0.03 Torr.
Aufarbeitung
- temperatureis heated
- temperatureat reflux for 16 hours under nitrogen gasification
- extractionexhaustively extracted with hexane
- washThe combined hexane extracts are washed with sodium bicarbonate solution and water
- dry with materialdried over sodium sulphate
- customevaporated
- distillationBy distillation there
Quellen und Nachweise
- ORD-Eintrag
- ord-371e8a1fcf7f4418af5fe2f16400894e
- Quelldatensatz
- uspto-grants-1980_12
- Patentnummer
- US04241058
Verknüpfte Notizen
Wird geladen…