Methanol → 4,4,4-Trifluoro-2,2-dimethylbutan-1-ol

HRID 1616246Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1616246
[F:1][C:2]([F:13])([F:12])[CH2:3][C:4]([CH3:11])([CH3:10])[C:5](OCC)=[O:6].[H-].[H-].[H-].[H-].[Li+].[Al+3].CO>CCOCC>[F:1][C:2]([F:13])([F:12])[CH2:3][C:4]([CH3:11])([CH3:10])[CH2:5][OH:6]

Komponenten

5

Edukt 3

HCID 887MethanolHCID 9990309Ethyl 2,2-dimethyl-4,4,4-trifluorobutanoateHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 597069974,4,4-Trifluoro-2,2-dimethylbutan-1-ol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

To a solution of ethyl 4,4,4-trifluoro-2,2-dimethylbutanoate (1 g, 5.05 mmol) in ether (25 ml) under nitrogen was added LAH (1M solution in ether, 20.2 mmol) and allowed to stir at room temperature for one hour. Methanol was slowly added to R×n until bubbling stopped. The reaction was then suspended in ether and Water. The suspension was washed with Water, dried over sodium sulfate, filtered, and concentrated without heat to produce an oil 4,4,4-trifluoro-2,2-dimethylbutan-1-ol (75-1). 1H NMR (500 MHz, CDCl3) δ 3.4 (s, 2H), 2.20-2.01 (m, 2H), 1.05 (s, 6H). (M+H)+: observed=157.16, calculated=157.15

Aufarbeitung

  1. customuntil bubbling
  2. washThe suspension was washed with Water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. temperaturewithout heat

Quellen und Nachweise

ORD-Eintrag
ord-acc82fe7a09441d99dc41e8240c65117
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08765784B2

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