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

HRID 2117470노트

반응식

HRID 2117470 반응식
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

참가 물질

4

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c5ba019d84af421a995cbf47d2880229
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07442702B2

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