Sodium Hydroxide → 3-(4-Tert.butyl-cyclohexyl)-2-methyl-allyl alcohol
Reaktionsgleichung
C([O:3][C:4](=O)[C:5]([CH3:17])=[CH:6][CH:7]1[CH2:12][CH2:11][CH:10]([C:13]([CH3:16])([CH3:15])[CH3:14])[CH2:9][CH2:8]1)C.[OH-].[Na+]>C1(C)C=CC=CC=1>[C:13]([CH:10]1[CH2:9][CH2:8][CH:7]([CH:6]=[C:5]([CH3:17])[CH2:4][OH:3])[CH2:12][CH2:11]1)([CH3:16])([CH3:14])[CH3:15]Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 40 °C
Versuchsvorschrift
46 g. of a 70% sodium dihydro-bis(2-methoxyethoxy)-aluminate solution in toluene are added dropwise at 25°-30° C. over a period of 90 minutes to a solution of 25.3 g of 3-(4-tert.butyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester in 130 ml of absolute toluene and the mixture is subsequently warmed at 40° C. for 2 hours. The mixture is then cooled down to -10° C., treated dropwise with 130 ml of 2-N sodium hydroxide, the toluene phase is separated and the aqueous-alkaline phase is back-extracted twice with 200 ml of toluene. The combined toluene phases are washed neutral with water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 3-(4-tert.butyl-cyclohexyl)-2-methyl-allyl alcohol of boiling point 112°-114° C./0.08 Torr.
Aufarbeitung
- temperatureThe mixture is then cooled down to -10° C.
- customthe toluene phase is separated
- extractionthe aqueous-alkaline phase is back-extracted twice with 200 ml of toluene
- washThe combined toluene phases are washed neutral with water
- dry with materialdried over sodium sulphate
- customevaporated
- distillationBy distillation there
Quellen und Nachweise
- ORD-Eintrag
- ord-e977be08e5b04de0adb1a4c9441075ab
- Quelldatensatz
- uspto-grants-1980_12
- Patentnummer
- US04241058
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