反应详情

A solution of 2-chloronicotinic acid (1.61 g, 10.2 mmol) and sulfuric acid (0.5 mL) in methanol (30 mL) was stirred at reflux overnight. The solution was poured into water (100 mL) and neutralised with NaHCO3 (s) before being extracted with 1:1 hexane/ethyl acetate (3×40 mL). The solvents were dried (MgSO4) and evaporated and the residue was purified by flash column chromatography (SiO2, 25% ethyl acetate/hexane eluent) to afford the ester as a colourless oil (700 mg, 40%).

1. temperatureat reflux overnight
2. extractionbefore being extracted with 1:1 hexane/ethyl acetate (3×40 mL)
3. dry with materialThe solvents were dried (MgSO4)
4. customevaporated
5. customthe residue was purified by flash column chromatography (SiO2, 25% ethyl acetate/hexane eluent)