Sodium Hydroxide → 5-(3-((3-(3-Chloro-phenyl)-propyl)-(Pyridine-3-sulfonyl)-amino)-propyl)-thiophene-2-carboxylic acid

HRID 2117470ノート

反応式

HRID 2117470 の反応式
C[O:2][C:3]([C:5]1[S:6][C:7]([CH2:10][CH2:11][CH2:12][N:13]([CH2:23][CH2:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[CH:27]=2)[S:14]([C:17]2[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=2)(=[O:16])=[O:15])=[CH:8][CH:9]=1)=[O:4].[OH-].[Na+]>CCO>[Cl:32][C:28]1[CH:27]=[C:26]([CH2:25][CH2:24][CH2:23][N:13]([S:14]([C:17]2[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=2)(=[O:16])=[O:15])[CH2:12][CH2:11][CH2:10][C:7]2[S:6][C:5]([C:3]([OH:4])=[O:2])=[CH:9][CH:8]=2)[CH:31]=[CH:30][CH:29]=1

参加物

4

実験手順

A solution of 5-(3-((3-(3-chloro-phenyl)-propyl)-(pyridine-3-sulfonyl)-amino)-propyl)-thiophene-2-carboxylic acid methyl ester prepared of Example 4, Step B (0.119 g, 0.241 mmol), in 5 mL EtOH and 0.72 mL 1N NaOH was stirred at room temperature overnight. The reaction mixture was adjusted to pH 6.2 and the layers were separated. The organic solution was washed with water, dried over MgSO4, filtered and concentrated in vacuo to afford the title compound (16 mg). 1H NMR (400 MHz, CDCl3) δ 8.00 (d, 1H, J=8), 7.70 (d, 1H, J=4), 7.30-7.60 (m, 6H), 6.75 (d, 1, J=4), 3.20 (m, 4H), 2.95 (t, 2H, J=7), 2.60 (t, 2H, J=7), 1.70-2.00 (m, 4H); MS 478 (M+1), 476 (M−1).

後処理

  1. customthe layers were separated
  2. washThe organic solution was washed with water
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c5ba019d84af421a995cbf47d2880229
出典データセット
uspto-grants-2008_10
特許番号
US07442702B2

反応ノート

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