Sodium Sulfate → 2-(4-Benzyloxy-phenyl)-ethylamine

HRID 850453

반응식

HRID 850453 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH2:7]([O:14][C:15]1[CH:20]=[CH:19][C:18]([CH2:21][C:22]#[N:23])=[CH:17][CH:16]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH2:7]([O:14][C:15]1[CH:16]=[CH:17][C:18]([CH2:21][CH2:22][NH2:23])=[CH:19][CH:20]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

5

반응물 3

HCID 24436Sodium SulfateHCID 5228044-BenzyloxyphenylacetonitrileHCID 21226445Aluminium lithium hydride

생성물 1

HCID 2009572-(4-Benzyloxy-phenyl)-ethylamine수율 17.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

LAH (2.82 g, 0.15 mol, 1.5 eq) was dissolved in THF (50 ml), and to this solution was added dropwise a THF solution (50 ml) of 4-benzyloxyphenyl-acetonitrile (11.1 g, 0.05 mol, 1.0 eq) under ice-cooling. After the completion of the dropwise addition, the mixture was refluxed under heating for 1.5 hours. The reaction mixture was cooled to room temperature, and a saturated aqueous sodium sulfate solution (about 40 ml) was added under ice-cooling. After filtration through Celite, the filtrate was concentrated under reduced pressure. The obtained residue was purified by column chromatography (chloroform/methanol=10/1) to give 2-(4-benzyloxyphenyl)ethylamine (2.02 g, 17.9%) as colorless needles.

후처리

  1. temperaturecooling
  2. additionAfter the completion of the dropwise addition
  3. temperaturethe mixture was refluxed
  4. temperatureunder heating for 1.5 hours
  5. temperaturecooling
  6. filtrationAfter filtration through Celite
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe obtained residue was purified by column chromatography (chloroform/methanol=10/1)

출처 및 근거

ORD 기록
ord-c3d6b82f3fc54961b9ea1904b810bbd8
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06017919

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