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

HRID 1616246ノート

反応式

HRID 1616246 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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

後処理

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

出典と根拠

ORDレコード
ord-acc82fe7a09441d99dc41e8240c65117
出典データセット
uspto-grants-2014_07
特許番号
US08765784B2

反応ノート

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