Ethyl cyanoacetate → HCID 86667498, compound

Participants

Reaction Steps

To a solution obtained by dissolving 24.0 g (1.04 mol) of sodium metal in 400 ml of ethanol, 113.1 g (1.00 mol) of ethyl cyanoacetate was dropwise added with stirring at the room temperature. After stirring for one hour, 150.0 g (1.05 mol) of ethyl trifluoroacetate was dropwise added to the reaction mixture and stirred for 3 hours at the same temperature. After finishing the reaction, the reaction mass was concentrated as intact under reduced pressure. Precipitated solid was the desired product. Ethyl 2-cyano-3-hydroxy-4,4,4-trifluoro-2-butenoate sodium salt thus obtained was 221.86 g. The yield was 96 %. Following results were obtained by NMR analysis. 1H-NMR (acetone-d6, bppm): 1.21(3H, t, J=6.9 Hz), 4.09(2H, q, J=6.9 Hz)

Provenance & Evidence