Methanol → 5-Bromo-6-methoxy-3-pyridinecarboxylic acid

HRID 1475723노트

반응식

HRID 1475723 반응식
C[O:2][C:3](=[O:13])[C:4]1[CH:9]=[C:8]([Br:10])[C:7]([O:11][CH3:12])=[N:6][CH:5]=1.[OH-].[Li+].CO>O1CCOCC1.O>[Br:10][C:8]1[C:7]([O:11][CH3:12])=[N:6][CH:5]=[C:4]([CH:9]=1)[C:3]([OH:13])=[O:2]

참가 물질

6

반응물 3

HCID 887MethanolHCID 3939Lithium HydroxideHCID 46311221Methyl 5-bromo-6-methoxypyridine-3-carboxylate

생성물 1

HCID 457904665-Bromo-6-methoxy-3-pyridinecarboxylic acid

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

반응 조건

온도
60 °C

실험 절차

5-Bromo-6-methoxy-nicotinic acid methyl ester (W. J. Thompson et al., J. Org. Chem. 49 (1984), 5237-5243; 2.00 g, 8.13 mmol) was dissolved in dioxane (40 ml), lithium hydroxide (40 ml of a 1 M solution in water) was added and subsequently sufficient methanol to achieve complete dissolution. The mixture was stirred at 60° C. for 2 h. The methanol was evaporated in vacuo and the remaining mixture was acidified with 2 N hydrochloric acid and extracted with EA. The combined extracts were dried over sodium sulfate, filtered and evaporated to dryness to yield the title compound.

후처리

  1. dissolutiondissolution
  2. customThe methanol was evaporated in vacuo
  3. extractionextracted with EA
  4. dry with materialThe combined extracts were dried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-55992b6fb1d943c5ac0348aed49c4555
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09018383B2

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