Sodium Hydroxide → 6-[(3-{[(Benzyloxy)carbonyl](methyl)amino}propyl)(methyl)carbamoyl]pyridine-3-carboxylic acid
反応式
[CH2:1]([O:8][C:9]([N:11]([CH3:29])[CH2:12][CH2:13][CH2:14][N:15]([CH3:28])[C:16]([C:18]1[N:23]=[CH:22][C:21]([C:24]([O:26]C)=[O:25])=[CH:20][CH:19]=1)=[O:17])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>CO>[CH2:1]([O:8][C:9]([N:11]([CH3:29])[CH2:12][CH2:13][CH2:14][N:15]([CH3:28])[C:16]([C:18]1[N:23]=[CH:22][C:21]([C:24]([OH:26])=[O:25])=[CH:20][CH:19]=1)=[O:17])=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1参加物
4
反応条件
- 温度
- 50 °C
実験手順
The compound (1.23 g, 3.08 mmol) obtained in Example 5a was dissolved in methanol (9 mL), a 1 N aqueous sodium hydroxide solution (9.24 mL, 9.24 mmol) was added, and then the mixture was stirred at 50° C. for 10 hours. The solvent was evaporated under reduced pressure, ethyl acetate was added to the resulting residue, the mixture was extracted with water (×2), the aqueous layer was adjusted to pH 3 with 1 N hydrochloric acid, and the mixture was extracted with methylene chloride (×3) and dried with anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the title compound (799 mg; yield, 68%) as a colorless oily substance.
後処理
- customThe solvent was evaporated under reduced pressure, ethyl acetate
- additionwas added to the resulting residue
- extractionthe mixture was extracted with water (×2)
- extractionthe mixture was extracted with methylene chloride (×3)
- dry with materialdried with anhydrous sodium sulfate
- customThe solvent was evaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-b8efe9554d574af5a563aa38c1618614
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08476253B2
反応ノート
読み込み中…