反应详情

温度

90 °C

To 20 ml of chloroform solution of ethyl 3-ethoxy-2-pentafluorobenzoylacrylate prepared from 5.6 g of ethyl 2,3,4,5,6-pentafluorobenzoylacetate by normal process was added 2-amino-3,5-difluoro-6-(p-methoxybenzylamino)pyridine until the disappearance of the ethyl acrylate spot in TLC analysis. The solution was concentrated under reduced pressure. To the residue were added 4.3 g of anhydrous potassium carbonate and 15 ml of N,N-dimethylformamide, and the mixture was stirred at 90° C. for 15 minutes and allowed to cool. The solution was separated by adding 100 ml of chloroform and 1 liter of distilled water, and the chloroform layer was washed twice with 1 liter of distilled water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The precipitate was dispersed in ethanol, collected by filtration, and washed with ethanol and diisopropylether successively to obtain 6.15 g of the title compound as a colorless powder.

1. concentrationThe solution was concentrated under reduced pressure
2. additionTo the residue were added 4.3 g of anhydrous potassium carbonate and 15 ml of N,N-dimethylformamide
3. temperatureto cool
4. customThe solution was separated
5. additionby adding 100 ml of chloroform and 1 liter of distilled water
6. washthe chloroform layer was washed twice with 1 liter of distilled water
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. additionThe precipitate was dispersed in ethanol
10. filtrationcollected by filtration
11. washwashed with ethanol and diisopropylether successively