Water → 3-Phenylcyclohexan-1-amine

HRID 1021520노트

반응식

HRID 1021520 반응식
[C:1]1([CH:7]2[CH2:12][CH2:11][CH2:10][C:9](=[N:13]O)[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1.CCOC(C)=O>[C:1]1([CH:7]2[CH2:12][CH2:11][CH2:10][CH:9]([NH2:13])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

7

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 866532373-Phenylcyclohexanone oxime

생성물 1

HCID 30281283-Phenylcyclohexan-1-amine수율 74%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 3-phenylcyclohexanone oxime (0.060 g, 0.32 mmol) in THF (2 ml) was added 1M lithium aluminum hydride in THF (0.67 ml, 0.67 mmol), and the reaction was heated to reflux for 3 hours. The reaction was cooled to ambient temperature and water (0.0254 ml), 1M sodium hydroxide (0.0254 ml), and additional water (0.0762 ml) were added sequentially, and the reaction was stirred for 15 minutes. The reaction was diluted with EtOAc and filtered. The filtrate was concentrated to yield 41 mg of the title compound (74% yield).

후처리

  1. temperaturethe reaction was heated
  2. temperatureto reflux for 3 hours
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-c3d811e15b784873a81460d509f7ddd4
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716498B2

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