Sodium Hydroxide → 2-[4-(3-Methylamino-piperidin-1-yl)-phenyl]-6-[(S)-1-(tetrahydrofuran-2-yl)methoxy]-2H-isoquinolin-1-one

HRID 69491노트

반응식

HRID 69491 반응식
[CH3:1][N:2]([CH:6]1[CH2:11][CH2:10][CH2:9][N:8]([C:12]2[CH:17]=[CH:16][C:15]([N:18]3[CH:27]=[CH:26][C:25]4[C:20](=[CH:21][CH:22]=[C:23]([O:28][CH2:29][C@@H:30]5[CH2:34][CH2:33][CH2:32][O:31]5)[CH:24]=4)[C:19]3=[O:35])=[CH:14][CH:13]=2)[CH2:7]1)C(=O)C.[OH-].[Na+]>S(=O)(=O)(O)O>[CH3:1][NH:2][CH:6]1[CH2:11][CH2:10][CH2:9][N:8]([C:12]2[CH:17]=[CH:16][C:15]([N:18]3[CH:27]=[CH:26][C:25]4[C:20](=[CH:21][CH:22]=[C:23]([O:28][CH2:29][C@@H:30]5[CH2:34][CH2:33][CH2:32][O:31]5)[CH:24]=4)[C:19]3=[O:35])=[CH:14][CH:13]=2)[CH2:7]1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 57916875N-methyl-N-[1-(4-{1-oxo-6-[(S)-1-(tetrahydrofuran-2-yl)methoxy]-1H-isoquinolin-2-yl}-phenyl)-piperidin-3-yl]-acetamide

생성물 1

HCID 579167212-[4-(3-Methylamino-piperidin-1-yl)-phenyl]-6-[(S)-1-(tetrahydrofuran-2-yl)methoxy]-2H-isoquinolin-1-one

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A solution of N-methyl-N-[1-(4-{1-oxo-6-[(S)-1-(tetrahydrofuran-2-yl)methoxy]-1H-isoquinolin-2-yl}-phenyl)-piperidin-3-yl]-acetamide (552 mg) was stirred in 20% sulfuric acid (with methanol as solubilizing agent) for 16 h at 90° C. The mixture was neutralized with 2N NaOH, extracted with dichloromethane, dried over magnesium sulfate and concentrated. The residue was purified by preparative HPLC. In this way the product was obtained with molecular weight 433.56 (C26H31N3O3); MS (ESI): 434 (M+H+).

후처리

  1. extractionextracted with dichloromethane
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by preparative HPLC
  5. customIn this way the product was obtained with molecular weight 433.56 (C26H31N3O3)

출처 및 근거

ORD 기록
ord-27f10a5e0f7143eaaa831baff2736e28
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822495B2

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