1-Butanol → HCID 54574149, Verbindung
Reaktionsgleichung
[Na].[CH2:2]([O:4][C:5](=[O:17])[CH:6]=[C:7]([CH2:15][CH3:16])[CH:8]([CH3:14])[CH2:9][CH:10]=[C:11]([CH3:13])[CH3:12])[CH3:3].[CH2:18](O)[CH2:19]CC>C(O)(=O)C>[CH2:2]([O:4][C:5](=[O:17])[CH:6]=[C:7]([CH2:15][CH3:16])[CH:8]([CH3:14])[CH2:9][CH:10]=[C:11]([CH3:12])[CH3:13])[CH2:3][CH2:18][CH3:19]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
A solution of 100 mg of sodium in 85 ml of n-butanol is placed in a flask filled with nitrogen and cooled to ca 5° C. At this temperature, 20 g (0.09 mol) of 3-ethyl-4,7-dimethyl-2,6-octadienoic acid ethyl ester are added. The mixture is then warmed to 60° C for 5 hours and to 100° C for 3 hours. For the working-up, the mixture is acidified with a few drops of glacial acetic acid and then the major part of the n-butanol is distilled off on a rotary evaporator. The residue is taken up in n-hexane, washed twice with sodium bicarbonate solution and three times with water, dried over sodium sulphate and evaporated. The crude product (19.3 g) is fractionally distilled. There are obtained 16.4 g (73%) of pure 3-ethyl-4,7-dimethyl-2,6-octadienoic acid n-butyl ester of boiling point 90°-92° C/0.04 mm Hg; nD20 = 1.4677.
Aufarbeitung
- additionfilled with nitrogen
- temperaturecooled to ca 5° C
- distillationthe major part of the n-butanol is distilled off on a rotary evaporator
- washwashed twice with sodium bicarbonate solution and three times with water
- dry with materialdried over sodium sulphate
- customevaporated
- distillationThe crude product (19.3 g) is fractionally distilled
Quellen und Nachweise
- ORD-Eintrag
- ord-fee5b30617da41a797df337a1bcbbd48
- Quelldatensatz
- uspto-grants-1977_02
- Patentnummer
- US04006108
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