Diethyl (ethoxymethylene)malonate → HCID 13312968, compound

Participants

Reaction Conditions

Reaction Steps

2-amino-5-(3-pyridyl)-1,3,4-thiadiazole (10 g) was reacted with diethyl ethoxymethylene-malonate (18 g) under stirring at 120° C. for 9 hours. After cooling the reaction mixture was crystallized from CH2Cl2 -isopropyl ether to give diethyl N-[5-(3-pyridyl)-1,3,4-thiadiazol-2-yl]-aminomethylene-malonate, m.p. 144°-145° C. (15.8 g) which was treated with polyphosphoric acid (6.6 g: 3.5 g of 99% H3PO4 and 3.1 g of P2O5) and POCl3 (27.8 g) under stirring at 120° C. for 40 minutes.

Provenance & Evidence