Potassium Carbonate → HCID 178463141, compound

Participants

Reaction Steps

A mixture of 45.0 g of potassium carbonate and 50.0 g (272 mmol) of ethyl 4,4,4-trifluoroacetoacetate in 300 mL of ethanol was cooled with a salt/ice bath to about 0° C. and to this ethylhydrazine oxalate (44.9 g, 299 mmol) was added with a spatula with stirring. After 45 min (minutes) at about 0° C., the mixture was allowed to warm to ambient temperature and stir for 1 hour. It was then heated to reflux overnights The mixture was concentrated by evaporation under reduced pressure and the residue was diluted with dichloromethane and water. The product only partially dissolved and seemed to be distributed in both phases. The layers were separated and the aqueous layer was extracted with dichloromethane and filtered. The solids obtained on filtration were extracted with dichloromethane. The dichloromethane layers and extracts were combined, washed with water (2×200 mL), and dried and the volatiles were allowed to evaporate overnight. All of the solids were combined to obtain the title compound.

Provenance & Evidence