4-Benzyloxy-1-{2-oxo-2-[3-(2,2,2-trifluoro-acetyl)-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl]-ethyl}-1H-pyridin-2-one → 4-Hydroxy-1-{2-[3-(2,2,2-trifluoro-acetyl)-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl]-ethyl}-1H-pyridin-2-one

HRID 564084노트

반응식

HRID 564084 반응식
C([O:8][C:9]1[CH:14]=[CH:13][N:12]([CH2:15][C:16](=O)[C:17]2[CH:33]=[CH:32][C:20]3[CH2:21][CH2:22][N:23]([C:26](=[O:31])[C:27]([F:30])([F:29])[F:28])[CH2:24][CH2:25][C:19]=3[CH:18]=2)[C:11](=[O:35])[CH:10]=1)C1C=CC=CC=1>CO.Cl.[Pd]>[OH:8][C:9]1[CH:14]=[CH:13][N:12]([CH2:15][CH2:16][C:17]2[CH:33]=[CH:32][C:20]3[CH2:21][CH2:22][N:23]([C:26](=[O:31])[C:27]([F:28])([F:29])[F:30])[CH2:24][CH2:25][C:19]=3[CH:18]=2)[C:11](=[O:35])[CH:10]=1

참가 물질

5

반응물 1

HCID 580428744-Benzyloxy-1-{2-oxo-2-[3-(2,2,2-trifluoro-acetyl)-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl]-ethyl}-1H-pyridin-2-one

생성물 1

HCID 598220864-Hydroxy-1-{2-[3-(2,2,2-trifluoro-acetyl)-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl]-ethyl}-1H-pyridin-2-one

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 313Hydrochloric Acid용매HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

To 5.00 g (10.3 mmol) 4-benzyloxy-1-{2-oxo-2-[3-(2,2,2-trifluoro-acetyl)-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl]-ethyl}-1H-pyridin-2-one (preparation 21a) in 100 mL MeOH and 9.8 mL 1 M aqueous HCl-solution is added 500 mg of 10% Pd/C. The reaction mixture is stirred under a hydrogen atmosphere of 5000 hPa at 50° C. for 18 h. After filtration and evaporation of the solvent, is the residue purified by HPLC (Zorbax stable bond, C18; water (0.15% formic acid)/acetonitrile 95:5 to 5:95).

후처리

  1. filtrationAfter filtration and evaporation of the solvent
  2. custompurified by HPLC (Zorbax stable bond, C18; water (0.15% formic acid)/acetonitrile 95:5 to 5:95)

출처 및 근거

ORD 기록
ord-e646eb6962724d7cb52170bde82d6f38
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067590B2

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