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

HRID 69491ノート

反応式

HRID 69491 の反応式
[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

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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+).

後処理

  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)

出典と根拠

ORDレコード
ord-27f10a5e0f7143eaaa831baff2736e28
出典データセット
uspto-grants-2014_09
特許番号
US08822495B2

反応ノート

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