反应详情

温度

2.5 °C

A solution of 24.4 g of 2-chloro-5-fluoro-benzoyl chloride in 100 ml of dichloromethane was added dropwise to a solution of 26.8 g of aminomalonic acid diethyl ester hydrochloride and 38.6 ml of triethylamine in 50 ml of dichloromethane with cooling in an ice bath. The reaction mixture was stirred for 2 h while the temperature was maintained at 0-5° C. Then 100 ml of water were added slowly. The phases were separated, and the aqueous phase was extracted twice with 100 ml of dichloromethane. The combined organic phases were dried with sodium sulfate, filtered and evaporated to give 39.3 g of the crude title compound.

1. temperaturewith cooling in an ice bath
2. customThe phases were separated
3. extractionthe aqueous phase was extracted twice with 100 ml of dichloromethane
4. dry with materialThe combined organic phases were dried with sodium sulfate
5. filtrationfiltered
6. customevaporated