Ethanol → Ethyl 2-Chloro-6-methylisonicotinate
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
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
- temperatureat reflux for 2 hours
- customThe volatiles were removed by evaporation
- dissolutionthe residue was dissolved in methylene chloride
- washThe solution was washed with a saturated aqueous sodium hydrogen carbonate solution and brine
- dry with materialdried (MgSO4)
- customthe solvent removed by evaporation
- customThe residue was purified by column chromatography
- 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
反応ノート
読み込み中…