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Aluminium lithium hydride → 4-[1-(1,1,2,2,2-Pentafluoroethyl)-ethoxy]-benzylamine

HRID 2041500
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HRID 2041500 반응식
[F:1][C:2]([CH:8]([O:10][C:11]1[CH:18]=[CH:17][C:14]([C:15]#[N:16])=[CH:13][CH:12]=1)[CH3:9])([F:7])[C:3]([F:6])([F:5])[F:4].[H-].[Al+3].[Li+].[H-].[H-].[H-]>C(OCC)C>[F:1][C:2]([CH:8]([O:10][C:11]1[CH:12]=[CH:13][C:14]([CH2:15][NH2:16])=[CH:17][CH:18]=1)[CH3:9])([F:7])[C:3]([F:4])([F:6])[F:5]
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참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 576564594-[1-(1,1,2,2,2-Pentafluoroethyl)-ethoxy]-benzonitrile

생성물 1

HCID 576559984-[1-(1,1,2,2,2-Pentafluoroethyl)-ethoxy]-benzylamine수율 98%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Add (±)-4-[1-(1,1,2,2,2-pentafluoroethyl)-ethoxy]-benzonitrile (1 g, 3.8 mmol) to a slurry of lithium aluminum hydride (400 mg, 10 mmol) in diethyl ether (30 mL) at 0° C. under a nitrogen atmosphere. Stir the mixture at ambient temperature for 2 h, and then quench the reaction sequentially with water (1 mL) and 5N sodium hydroxide (1 mL). Filter the slurry through Celite®, dry the filtrate over Na2SO4, filter and concentrate in vacuo to obtain the title compound (990 mg, 98%). GC-MS m/z: 268 (M+).

후처리

  1. customquench
  2. customthe reaction sequentially with water (1 mL) and 5N sodium hydroxide (1 mL)
  3. filtrationFilter the slurry through Celite®
  4. dry with materialdry the filtrate over Na2SO4
  5. filtrationfilter
  6. concentrationconcentrate in vacuo

출처 및 근거

ORD 기록
ord-924def16cd664142ae463d8d4970f3bb
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08580780B2

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