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

HRID 80530노트

반응식

HRID 80530 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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)+.

후처리

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

출처 및 근거

ORD 기록
ord-6d398277ccd144f1a35fda823db8d6fe
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846663B2

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