Sodium Bicarbonate → HCID 18426828, 화합물

HRID 1281152노트

반응식

HRID 1281152 반응식
[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

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 521998p-Toluenesulfonic acid monohydrateHCID 18426809HCID 18426809, 화합물

생성물 1

HCID 18426828HCID 18426828, 화합물수율 92%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-5013da4bf20f4081a5568b4613bb4517
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06452014B1

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