Reaktionsgleichung
C([Li])CCC.Br[C:7]1[CH:12]=[CH:11][C:10]([C:13]([O:17][CH3:18])([O:15][CH3:16])[CH3:14])=[CH:9][CH:8]=1.[CH3:19][C:20]1([CH3:26])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1.[O:27]1CCCC1>C1CCCCC1>[CH3:16][O:15][C:13]([C:10]1[CH:11]=[CH:12][C:7]([C:23]2([OH:27])[CH2:24][CH2:25][C:20]([CH3:26])([CH3:19])[CH2:21][CH2:22]2)=[CH:8][CH:9]=1)([O:17][CH3:18])[CH3:14]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- -78 °C
Versuchsvorschrift
328 ml of a 1.6 M solution of butyllithium in cyclohexane are added at −78° C. to 117 g of 1-bromo-4-(1,1-dimethoxyethyl)benzene in 1100 ml of tetrahydrofuran and the reaction mixture is stirred at −78° C. for 2 hours. 66 g of 4,4-dimethylcyclohexane dissolved in 210 ml of tetrahydrofuran are added at this same temperature and the reaction mixture is stirred for 1 hour at −78° C. The reaction mixture is hydrolysed by addition of crushed ice. The organic phase is separated out after settling of the phases has taken place, it is dried over sodium sulphate and the solvents are evaporated off under reduced pressure. The compound obtained is recrystallized from 500 ml of n-hexane; m.p.=88° C.
Aufarbeitung
- additionare added at this same temperature
- stirringthe reaction mixture is stirred for 1 hour at −78° C
- additionThe reaction mixture is hydrolysed by addition of crushed ice
- customThe organic phase is separated out
- dry with materialis dried over sodium sulphate
- customthe solvents are evaporated off under reduced pressure
- customThe compound obtained
- customis recrystallized from 500 ml of n-hexane
Quellen und Nachweise
- ORD-Eintrag
- ord-44b86795716e4ad79350c88828f2e8e9
- Quelldatensatz
- uspto-grants-2002_11
- Patentnummer
- US06482986B1
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