Ethanol → Ethyl 2-Chloro-6-methylisonicotinate

HRID 279570

反応式

HRID 279570 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 22625009Ethyl 2-Chloro-6-methylisonicotinate収率 86%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-aa3c537a6ce2407e9bec13fb8511e4c7
出典データセット
uspto-grants-2002_03
特許番号
US06362336B1

関連ノート

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