Boron trifluoride etherate → 2-(1-Cyclohexylethoxy)-2-methyl-1-propanol
Reaktionsgleichung
B(F)(F)F.O(CC)CC.[CH:10]1([CH:16]([OH:18])[CH3:17])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1.[CH3:19][C:20]1([O:23][CH2:22]1)[CH3:21]>C1CCCCC1>[CH:10]1([CH:16]([O:18][C:20]([CH3:21])([CH3:19])[CH2:22][OH:23])[CH3:17])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
BF3—OEt2 (2.0 ml) is added dropwise to a solution of 1-cyclohexylethanol (16.6 g, 127.0 mmol) and isobutylene oxide (2.9 g, 40.0 mmol) in cyclohexane (20 ml) that has been cooled to 0° C. The reaction mixture is now stirred at 0° C. for a further 30 minutes, and further, BF3—OEt2 (2.0 ml) is then added. After a further 3 hours at 0° C., the cooling is removed and the reaction solution is washed once with 1 M NaOH (15 ml). The organic phase is dried over Na2SO4, filtered off and freed from solvent in a rotary evaporator. The 1-cyclohexylethanol that has not completely reacted is removed from the crude product; thus, obtained by means of bulb tube distillation (BTD) and 5.3 g crude 2-(1-cyclohexylethoxy)-2-methyl-1-propanol is obtained which has a GC content of 75% and can be used in the next reaction without further purification.
Aufarbeitung
- waitAfter a further 3 hours at 0° C.
- customthe cooling is removed
- washthe reaction solution is washed once with 1 M NaOH (15 ml)
- dry with materialThe organic phase is dried over Na2SO4
- filtrationfiltered off
- customfreed from solvent in a rotary evaporator
- customThe 1-cyclohexylethanol that has not completely reacted
- customis removed from the crude product
- customthus, obtained by means of bulb tube
- distillationdistillation (BTD)
Quellen und Nachweise
- ORD-Eintrag
- ord-27d36f7e05ac4c0799ed0dd01f66ed6f
- Quelldatensatz
- uspto-grants-2006_06
- Patentnummer
- US07064102B2
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