Ethanol → Ethyl 2-Chloro-6-methylisonicotinate
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]=1참가 물질
4
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
- 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)
출처 및 근거
- ORD 기록
- ord-aa3c537a6ce2407e9bec13fb8511e4c7
- 출처 데이터셋
- uspto-grants-2002_03
- 특허 번호
- US06362336B1
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