Methanol → HCID 46311240、化合物

HRID 384117ノート

反応式

HRID 384117 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[C:5]([F:11])=[CH:4][CH:3]=1.[OH-].[Na+].[CH3:14]O>S(=O)(=O)(O)O>[CH3:14][O:9][C:8]([C:6]1[C:5]([F:11])=[CH:4][CH:3]=[C:2]([Cl:1])[N:7]=1)=[O:10]

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 447547876-Chloro-3-fluoropyridine-2-carboxylic acid

生成物 1

HCID 46311240HCID 46311240、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

To a solution of 6-chloro-3-fluoropyridin-2-carboxylic acid (250 mg) in methanol (3 ml), 0.3 ml of concentrated sulfuric acid was added, and the reaction solution was heated to reflux for 2.5 hours. The reaction solution was cooled, and then the solvent was distilled off under reduced pressure. To the residue obtained was added 1N aqueous sodium hydroxide, and the mixture was extracted with ethyl acetate. The combined organic layers were washed with a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to afford the title compound as a white solid.

後処理

  1. temperaturethe reaction solution was heated
  2. temperatureto reflux for 2.5 hours
  3. temperatureThe reaction solution was cooled
  4. distillationthe solvent was distilled off under reduced pressure
  5. customTo the residue obtained
  6. extractionthe mixture was extracted with ethyl acetate
  7. washThe combined organic layers were washed with a saturated saline solution
  8. dry with materialdried over anhydrous sodium sulfate
  9. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-f3b65c4193f94445984acb887c6a9c9b
出典データセット
uspto-grants-2013_02
特許番号
US08367708B2

反応ノート

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