Water → 3-Phenylcyclohexan-1-amine

HRID 1021520ノート

反応式

HRID 1021520 の反応式
[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

参加物

7

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 866532373-Phenylcyclohexanone oxime

生成物 1

HCID 30281283-Phenylcyclohexan-1-amine収率 74%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-c3d811e15b784873a81460d509f7ddd4
出典データセット
uspto-grants-2014_05
特許番号
US08716498B2

反応ノート

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