Methanol → Methyl 5-bromopyridine-3-carboxylate

HRID 52837

反応式

HRID 52837 の反応式
[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

参加物

4

反応物 2

HCID 887MethanolHCID 887075-Bromonicotinic acid

生成物 1

HCID 699336Methyl 5-bromopyridine-3-carboxylate

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-482055b3c6d947c9bccd28c18aa9d287
出典データセット
uspto-grants-1997_04
特許番号
US05616714

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