Diethyl (ethoxymethylene)malonate → HCID 4048131, compound

Participants

Reaction Steps

2-amino-1,3,4-thiadiazole (5 g) was reacted with diethyl ethoxymethylenemalonate (26.5 g) in ethanol (20 ml) at the reflux temperature for 23 hours. After cooling the precipitate was filtered and purified with hexane to give diethyl N-(1,3,4-thiadiazol-2-yl)-aminomethylenemalonate, m.p. 107°-111° C. (10 g), which was treated with polyphosphoric acid (57.6 g; 30.8 g of 99% H3PO4 and 26.8 g of P2O5) and POCl3 (25 g) under stirring at 120° C. for 30 minutes.

Provenance & Evidence