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

HRID 82481

반응식

HRID 82481 반응식
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]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028Tetrahydrofuran2회HCID 673472813-Methyl-2-[pyridine-3-carbonyl-amino]-pentanoic acid methyl ester

생성물 1

HCID 167765993-Methyl-2-[pyridine-3-carbonyl-amino]-pentanoic acid수율 50.2%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 962Water용매

반응 조건

온도
25 °C

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-7d62649520f64d96b695ecfb33956a17
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846721B2

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