Sodium Hydroxide → 5-(3-((3-(3-Chloro-phenyl)-propyl)-(Pyridine-3-sulfonyl)-amino)-propyl)-thiophene-2-carboxylic acid
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
反応物 2
生成物 1
試薬・触媒・溶媒 1
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, 1H, 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
- customthe layers were separated
- washThe organic solution was washed with water
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-a80e7a43b16345f1b7cf09e07281c5b3
- 出典データセット
- uspto-grants-2002_12
- 特許番号
- US06498172B1
反応ノート
読み込み中…