Ethanol → Ethyl 2-Chloro-6-methylisonicotinate

HRID 279570

반응식

HRID 279570 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[C:4]([CH3:11])[N:3]=1.[CH2:12](O)[CH3:13]>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([O:10][CH2:12][CH3:13])=[O:9])[CH:5]=[C:4]([CH3:11])[N:3]=1

참가 물질

4

반응물 2

HCID 702EthanolHCID 1412092-Chloro-6-methylpyridine-4-carboxylic acid

생성물 1

HCID 22625009Ethyl 2-Chloro-6-methylisonicotinate수율 86%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A solution of 2-chloro-6-methyl-4-pyridinecarboxylic acid (2 g, 12 mmol) in ethanol (100 ml) and concentrated sulphuric acid (10 ml) was heated at reflux for 2 hours. The volatiles were removed by evaporation and the residue was dissolved in methylene chloride. The solution was washed with a saturated aqueous sodium hydrogen carbonate solution and brine, dried (MgSO4) and the solvent removed by evaporation. The residue was purified by column chromatography eluting with ethyl acetate/petroleum ether (1/9) to give ethyl 2-chloro-6-methyl-4-pyridinecarboxylate (2 g, 86%).

후처리

  1. temperatureat reflux for 2 hours
  2. customThe volatiles were removed by evaporation
  3. dissolutionthe residue was dissolved in methylene chloride
  4. washThe solution was washed with a saturated aqueous sodium hydrogen carbonate solution and brine
  5. dry with materialdried (MgSO4)
  6. customthe solvent removed by evaporation
  7. customThe residue was purified by column chromatography
  8. washeluting with ethyl acetate/petroleum ether (1/9)

출처 및 근거

ORD 기록
ord-aa3c537a6ce2407e9bec13fb8511e4c7
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06362336B1

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