Water → (2,3,4,5-tetrahydro-1H-1-benzazepin-2-yl)methanamine

HRID 1035309ノート

反応式

HRID 1035309 の反応式
[N+:1](/[CH:4]=[C:5]1\[NH:6][C:7]2[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=2[CH2:9][CH2:10][CH2:11]\1)([O-])=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>O1CCCC1>[NH:6]1[C:7]2[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=2[CH2:9][CH2:10][CH2:11][CH:5]1[CH2:4][NH2:1]

参加物

5

反応物 3

HCID 962WaterHCID 13842538(2z)-2-(Nitromethylene)-2,3,4,5-tetrahydro-1h-1-benzazepineHCID 21226445Aluminium lithium hydride

生成物 1

HCID 13842540(2,3,4,5-tetrahydro-1H-1-benzazepin-2-yl)methanamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of Example 182D (0.643 g, 3.15 mmol) in tetrahydrofuran (31.5 mL) under argon was added dropwise lithium aluminum hydride in tetrahydrofuran (9.45 mL, 18.89 mmol), and the mixture was stirred at room temperature for 30 minutes. Water was added carefully and the mixture was extracted once with dichloromethane. The organic extract was dried over Na2SO4, and the solvent was evaporated to obtain the crude title compound which was used was used without purification for the next reaction. MS (ESI+) m/z 177.3 (M+H)+.

後処理

  1. extractionthe mixture was extracted once with dichloromethane
  2. extractionThe organic extract
  3. dry with materialwas dried over Na2SO4
  4. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-bf9c9902712b468197a4d7c765d4957c
出典データセット
uspto-grants-2013_10
特許番号
US08546377B2

反応ノート

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