Lithium Hydroxide → 4-Methyl-2-[pyridine-3-carbonyl]-amino-pentanoic acid

HRID 82498ノート

反応式

HRID 82498 の反応式
C[O:2][C:3](=[O:18])[C:4]([NH2:17])([C:9]([C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1)=[O:10])[CH2:5][CH:6]([CH3:8])[CH3:7].C1COCC1.[Li+].[OH-]>CO.O>[CH3:7][CH:6]([CH3:8])[CH2:5][C:4]([NH2:17])([C:9]([C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1)=[O:10])[C:3]([OH:18])=[O:2]

参加物

6

反応物 3

HCID 3939Lithium HydroxideHCID 8028Tetrahydrofuran2 回HCID 67325240HCID 67325240、化合物

生成物 1

HCID 673256494-Methyl-2-[pyridine-3-carbonyl]-amino-pentanoic acid収率 60%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

To a solution of 4-methyl-2-[pyridine-3-carbonyl]-amino-pentanoic acid methyl ester (0.80 g, 3.3 mmol), in methanol (8 mL), THF (3 mL) was added LiOH (0.7 g, 16.9 mmol), dissolved in water (9 mL). The mixture was allowed to stir at room temperature (25° C.) over 2.5 h. Methanol and THF was stripped off from the reaction mass, acidified the reaction mass using 1.5NHCl (pH=1). Extracted the reaction mass with ethyl acetate (100 mL) thrice and dried over sodium sulphate and concentrated to obtain product as pale yellow solid (0.45 g, 60%).

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-ecb67ae1468d4f908c766e03ad58f2d8
出典データセット
uspto-grants-2014_09
特許番号
US08846721B2

反応ノート

読み込み中…