Methanol → 5-Bromo-2-(methoxycarbonyl)pyridine 1-oxide

HRID 709599ノート

反応式

HRID 709599 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:9]([OH:11])=[O:10])=[N+:6]([O-:8])[CH:7]=1.S(Cl)(Cl)=O.[CH3:16]O>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:9]([O:11][CH3:16])=[O:10])=[N+:6]([O-:8])[CH:7]=1

参加物

4

反応物 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 684639675-Bromo-2-carboxypyridine 1-oxide

生成物 1

HCID 684583815-Bromo-2-(methoxycarbonyl)pyridine 1-oxide

実験手順

To a solution of 5-bromo-2-carboxypyridine 1-oxide (19.6 g) in methanol (300 mL) was added dropwise thionyl chloride (37.1 g) at 0° C., and the mixture was heated under reflux for 1 hr. The reaction mixture was concentrated under reduced pressure and the residue was washed with ethyl acetate to give the title compound (22.0 g) as white crystals. This compound was used for the next step without further purification.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1 hr
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. washthe residue was washed with ethyl acetate

出典と根拠

ORDレコード
ord-ad8b050a741b46949338660ce9f82816
出典データセット
uspto-grants-2015_11
特許番号
US09181186B2

反応ノート

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