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

HRID 1616246노트

반응식

HRID 1616246 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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

후처리

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

출처 및 근거

ORD 기록
ord-acc82fe7a09441d99dc41e8240c65117
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765784B2

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