Aluminium lithium hydride → 3,3-Difluoro-cyclopentaneMethanol

HRID 15001노트

반응식

HRID 15001 반응식
[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

참가 물질

5

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 58024202HCID 58024202, 화합물

생성물 1

HCID 593409733,3-Difluoro-cyclopentaneMethanol

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3ec67cf4abdb426688e975825bd2c4be
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732440B2

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