反应详情

温度

60 °C

0.49 mol of diethyl malonate was added at 60° C. inside 2 hours to a mixture of 0.51 mol of NaH and 140 ml of 1,4-dioxane. The mixture was stirred for approximately 10 min at 60° C. and then 0.05 mol of Cu(I)Br was added. After 15 min, a mixture of 0.25 mol of 4-bromo-3-fluorotoluene and 10 ml of 1,4-dioxane was added. The reaction mixture was heated at 100° C. for approximately 15 hours and was then cooled to 15° C. After acidifying with 35 ml of 12N HCl at 15 to 20° C., the precipitate produced was filtered off. The filtrate was extracted and the organic phases, after separation, were dried and then freed from the solvent. 40 g of the title compound were obtained.

1. waitAfter 15 min
2. additionwas added
3. temperatureThe reaction mixture was heated at 100° C. for approximately 15 hours
4. temperaturewas then cooled to 15° C
5. customthe precipitate produced
6. filtrationwas filtered off
7. extractionThe filtrate was extracted
8. customthe organic phases, after separation
9. customwere dried