反应详情

To 60 ml of dichloromethane were added 21.0 g of 2,6-dichloro-5-fluoronicotinic acid, 10 ml of oxalylchloride, and 10 drops of N,N-dimethylformamide, and the mixture was stirred at room temperature for one day. The solvent and the excess reagents were distilled off under reduced pressure, and the residue was dissolved in 50 ml of chloroform. 10 ml of methanol was added dropwise to the solution, and the solution was stirred at room temperature for 60 minutes, and 15 g of anhydrous potassium carbonate was added to the solution and the solution was stirred for another 30 minutes. The solution was separated by adding 150 ml of chloroform and 150 ml of distilled water, and the chloroform layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 26.6 g of the title compound as a colorless crude oily residue.

1. distillationThe solvent and the excess reagents were distilled off under reduced pressure
2. dissolutionthe residue was dissolved in 50 ml of chloroform
3. addition10 ml of methanol was added dropwise to the solution
4. stirringthe solution was stirred at room temperature for 60 minutes
5. addition15 g of anhydrous potassium carbonate was added to the solution
6. stirringthe solution was stirred for another 30 minutes
7. customThe solution was separated
8. additionby adding 150 ml of chloroform and 150 ml of distilled water
9. dry with materialthe chloroform layer was dried over anhydrous magnesium sulfate
10. concentrationconcentrated under reduced pressure