反应详情

温度

90 °C

To 1 ml of chloroform solution of ethyl 3-ethoxy-2-(3-bromo-2,4,5-trifluorobenzoyl)acrylate prepared from 0.65 g of ethyl 3-bromo-2,4,5-trifluorobenzoylacetate by normal process was added 0.3 g of 2-amino-6-(t-butylamino)-5-fluoropyridine. The solution was concentrated under reduced pressure to obtain yellowish orange solid residue. To this residue were added 0.4 g of anhydrous potassium carbonate and 2 ml of N,N-dimethylformamide, and the mixture was stirred at 90° C. for 25 minutes and allowed to cool. The solution was separated by adding 25 ml of chloroform and 400 ml of distilled water, and the chloroform layer was washed with 400 ml of distilled water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. After adding 2 ml of ethanol, the solution was and allowed to stand. The precipitate was dispersed in ethanol and collected by filtration, and washed with ethanol and diisopropylether successively to obtain 0.53 g of the title compound as a pale yellow powder.

1. concentrationThe solution was concentrated under reduced pressure
2. customto obtain yellowish orange solid residue
3. temperatureto cool
4. customThe solution was separated
5. additionby adding 25 ml of chloroform and 400 ml of distilled water
6. washthe chloroform layer was washed with 400 ml of distilled water
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. additionAfter adding 2 ml of ethanol
10. additionThe precipitate was dispersed in ethanol
11. filtrationcollected by filtration
12. washwashed with ethanol and diisopropylether successively