反应详情

First 17.1 g of ethyl 3-diethylaminoacrylate are added dropwise and then 10.5 g of triethylamine are added to a solution of 22.75 g of 2,4-dichloro-5-fluorobenzoyl chloride in 80 ml of anhydrous dioxane, while cooling in ice and stirring. The mixture is stirred at room temperature for one hour, heated to boiling under reflux for 45 minutes, and the solvent is removed by distillation in vacuo, and the oily residue is taken up in methylene chloride/water. The phases are separated, and the aqueous solution is again extracted with methylene chloride. The combined organic phases are washed with water, dried with sodium sulphate, and the methylene chloride is removed in vacuo. 29 g of ethyl 3-diethylamino-2-(2,4-dichloro-5-fluorobenzoyl)acrylate are obtained as a brown oil.

1. temperaturewhile cooling in ice
2. stirringThe mixture is stirred at room temperature for one hour
3. temperatureheated
4. temperatureunder reflux for 45 minutes
5. customthe solvent is removed by distillation in vacuo
6. customThe phases are separated
7. extractionthe aqueous solution is again extracted with methylene chloride
8. washThe combined organic phases are washed with water
9. dry with materialdried with sodium sulphate
10. customthe methylene chloride is removed in vacuo