Aluminium lithium hydride → 3,3-Difluoro-cyclopentaneMethanol

HRID 15001ノート

反応式

HRID 15001 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]1([F:18])[CH2:12][CH2:11][CH:10]([C:13](OCC)=[O:14])[CH2:9]1>C1COCC1.C(OCC)C>[F:7][C:8]1([F:18])[CH2:12][CH2:11][CH:10]([CH2:13][OH:14])[CH2:9]1

参加物

5

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 58024202HCID 58024202、化合物

生成物 1

HCID 593409733,3-Difluoro-cyclopentaneMethanol

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

6.4 ml of a 1M solution of lithium aluminum hydride in THF are initially charged in 40 ml of diethyl ether. With ice cooling, 1.12 g of ethyl 3,3-difluoro-cyclopentanecarboxylate dissolved in 10 ml of diethyl ether are added dropwise under argon. After one hour, the cooling bath is removed, and the reaction mixture is stirred for another three hours. The reaction mixture is then poured onto ice-cold saturated ammonium chloride solution and filtered off over a filtration aid. The filtrate is washed with saturated NaHCO3 solution, dried over MgSO4 and concentrated under reduced pressure. This gives 625 mg of (3,3-difluorocyclopentyl)methanol.

後処理

  1. additionare added dropwise under argon
  2. customthe cooling bath is removed
  3. additionThe reaction mixture is then poured onto ice-cold saturated ammonium chloride solution
  4. filtrationfiltered off over a filtration aid
  5. washThe filtrate is washed with saturated NaHCO3 solution
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-3ec67cf4abdb426688e975825bd2c4be
出典データセット
uspto-grants-2010_06
特許番号
US07732440B2

反応ノート

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