反应详情

温度

55 °C

Diethyl malonate (0.49 mol) was added to a mixture of sodium hydride (0.51 mol) and 1,4-dioxane (140 ml) at 55 to 60° C. within 2 hours. A mixture of 1,4-dioxane (50 ml) and diethyl malonate (0.13 mol) was added. The mixture was stirred for 10 minutes at 55° C. and copper(I) bromide (0.05 mol) was added. After 15 min. a mixture of 2-bromo-1,3,5-trifluorobenzene (0.25 mol) and 1,4-dioxane (10 ml) was added. The reaction mixture was heated at 100° C. for 15 hours and cooled to 15° C. Hydrochloric acid (12N, 35 ml) was added slowly at 15 to 20° C. The precipitate was filtered off. The filtrate was extracted with diethylether. The organic Phase was separated, dried with anhydrous sodium sulphate and filtered. The filtrate was evaporated under reduced Pressure to yield the product.

1. additionwas added
2. additionwas added
3. temperatureThe reaction mixture was heated at 100° C. for 15 hours
4. temperaturecooled to 15° C
5. filtrationThe precipitate was filtered off
6. extractionThe filtrate was extracted with diethylether
7. customThe organic Phase was separated
8. dry with materialdried with anhydrous sodium sulphate
9. filtrationfiltered
10. customThe filtrate was evaporated under reduced Pressure
11. customto yield the product