Hydrochloric Acid → 3-Methyl-2-[pyridine-3-carbonyl-amino]-pentanoic acid

HRID 82481

反応式

HRID 82481 の反応式
C[O:2][C:3](=[O:18])[CH:4]([NH:9][C:10]([C:12]1[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=1)=[O:11])[CH:5]([CH3:8])[CH2:6][CH3:7].C1COCC1.[Li+].[OH-].Cl>CO.O>[CH3:8][CH:5]([CH2:6][CH3:7])[CH:4]([NH:9][C:10]([C:12]1[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=1)=[O:11])[C:3]([OH:18])=[O:2]

参加物

7

反応条件

温度
25 °C

実験手順

To a solution of 3-methyl-2-[pyridine-3-carbonyl-amino]-pentanoic acid methyl ester (1.5 g, 5.9 mmol), in methanol (10 mL), THF (9 mL), was added LiOH (1.25 g, 29.9 mmol) dissolved in water (3 mL). The mixture was allowed to stir at room temperature (25° C.) over 3 h. Methanol and THF was stripped off from the reaction mass, acidified the reaction mass using 1.5N HCl (pH=2-3). Extracted the reaction mass with ethyl acetate (100 mL) thrice and dried over sodium sulphate and concentrated to obtain product as pale yellow solid (0.7 g, 50%).

後処理

  1. extractionExtracted the reaction mass with ethyl acetate (100 mL) thrice
  2. dry with materialdried over sodium sulphate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-7d62649520f64d96b695ecfb33956a17
出典データセット
uspto-grants-2014_09
特許番号
US08846721B2

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