Methanol → Methyl 5-bromopyridine-3-carboxylate

HRID 52837

반응식

HRID 52837 반응식
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].[CH3:11]O>Cl>[CH3:11][O:8][C:7](=[O:9])[C:6]1[CH:10]=[C:2]([Br:1])[CH:3]=[N:4][CH:5]=1

참가 물질

4

반응물 2

HCID 887MethanolHCID 887075-Bromonicotinic acid

생성물 1

HCID 699336Methyl 5-bromopyridine-3-carboxylate

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

5-Bromo-nicotinic acid (5,00 g, 24.7 mmol) was dissolved in methanol (50 mL) and saturated with hydrochloric acid gas. The reaction mixture was allowed to stand for 2.5 days and then filtered. The filtrate was concentrated under reduced pressure and methylene chloride was added. The solution was washed with saturated sodium bicarbonate solution. The aqueous wash was back-extracted with methylene chloride (2x). The combined organic extracts were dried over magnesium sulfate and concentrated in vacuo to afford 5-bromo-nicotinic acid methyl ester (4.72 g).

후처리

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated under reduced pressure and methylene chloride
  3. additionwas added
  4. washThe solution was washed with saturated sodium bicarbonate solution
  5. washThe aqueous wash
  6. extractionwas back-extracted with methylene chloride (2x)
  7. dry with materialThe combined organic extracts were dried over magnesium sulfate
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-482055b3c6d947c9bccd28c18aa9d287
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616714

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