Sodium Bicarbonate → HCID 18426828、化合物

HRID 1281152ノート

反応式

HRID 1281152 の反応式
[Br:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([CH:9]=[O:10])=[CH:4][C:3]=1[CH3:11].O.[C:13]1(C)C=CC(S(O)(=O)=O)=CC=1.[C:24](=[O:27])(O)[O-].[Na+]>CO>[Br:1][C:2]1[C:3]([CH3:11])=[CH:4][C:5]([CH:9]([O:27][CH3:24])[O:10][CH3:13])=[C:6]([CH3:8])[N:7]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 521998p-Toluenesulfonic acid monohydrateHCID 18426809HCID 18426809、化合物

生成物 1

HCID 18426828HCID 18426828、化合物収率 92%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 6-bromo-2,5-dimethyl-3-pyridinecarboxaldehyde (378 g, 1.77 mmol) in methanol (25 mL) was added p-toluenesulfonic acid hydrate (342 mg, 1.80 mmol), and the mixture was heated at reflux for 1 h. Diluted aqueous sodium bicarbonate was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine and dried on anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to afford 2-bromo-5-dimethoxymethyl-3,6-dimethylpyridine (423 g, 92%).

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 1 h
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried on anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-5013da4bf20f4081a5568b4613bb4517
出典データセット
uspto-grants-2002_09
特許番号
US06452014B1

反応ノート

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