反应详情

To a suspension of 5-chlorosalicylic acid (500 g) in ethanol (2 L) was added concentrated sulphuric acid (40 ml) with stirring at room temperature. After the reaction mixture was refluxed for 12 hours, the solvent was evaporated under reduced pressure and the residue was dissolved in ethyl acetate. The organic layer was washed with 10% NaCl solution and 4% sodium hydrogen carbonate solution, and then evaporated under reduced pressure, dried over anhydrous magnesium sulphate. After filtration, the solvent was evaporated under reduced pressure to give the title compound (514 g, 88%) as a pale-yellow oil.

1. temperatureAfter the reaction mixture was refluxed for 12 hours
2. customthe solvent was evaporated under reduced pressure
3. dissolutionthe residue was dissolved in ethyl acetate
4. washThe organic layer was washed with 10% NaCl solution and 4% sodium hydrogen carbonate solution
5. customevaporated under reduced pressure
6. dry with materialdried over anhydrous magnesium sulphate
7. filtrationAfter filtration
8. customthe solvent was evaporated under reduced pressure