Sodium Hydroxide → HCID 71268658、化合物

HRID 929367ノート

反応式

HRID 929367 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8](S(CCC)(=O)=O)[S:9]([CH2:12][CH2:13][CH3:14])(=[O:11])=[O:10])=[CH:4][C:3]=1[C:21]([C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][CH:32]=1)[N:29]=[CH:28][CH:27]=[N:26]2)=[O:22].[OH-].[Na+]>CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][S:9]([CH2:12][CH2:13][CH3:14])(=[O:11])=[O:10])=[CH:4][C:3]=1[C:21]([C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][CH:32]=1)[N:29]=[CH:28][CH:27]=[N:26]2)=[O:22]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 71268570N-(4-fluoro-3-(quinoxaline-6-carbonyl)phenyl)-N-(propylsulfonyl)propane-1-sulfonamide

生成物 1

HCID 71268658HCID 71268658、化合物収率 89.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of N-(4-fluoro-3-(quinoxaline-6-carbonyl)phenyl)-N-(propylsulfonyl)propane-1-sulfonamide (50 mg, 0.10 mmol, 1.0 eq.) in MeOH (10 mL) was added NaOH aqueous solution (1 N, 0.22 mL, 0.22 mmol, 2.2 eq.). The resulting mixture was stirred at it for 1 h, then concentrated. The resulting residue was purified by flash column chromatography (PE/EA=1/1, v/v) to afford N-(4-fluoro-3-(quinoxaline-6-carbonyl)phenyl)propane-1-sulfonamide (33.4 mg, 89.5%). LRMS (M+H+) m/z calculated 374.1, found 374.1. 1H NMR (CDCl3, 400 MHz) δ 8.94-8.97 (dd, 2 H), 8.46-8.47 (m, 1 H), 8.31-8.34 (m, 1 H), 8.23-8.25 (m, 1 H), 7.50-7.54 (m, 1 H), 7.46-7.48 (m, 1 H), 7.19-7.23 (t, 1 H), 6.80 (s, 1 H), 3.10-3.14 (m, 2 H), 1.86-1.92 (m, 2 H), 1.04-1.08 (t, 3 H).

後処理

  1. concentrationconcentrated
  2. customThe resulting residue was purified by flash column chromatography (PE/EA=1/1

出典と根拠

ORDレコード
ord-8da6cc9cb2d24947bd7c9d9688194e68
出典データセット
uspto-grants-2016_03
特許番号
US09295671B2

反応ノート

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