HCID 67843395, compound → HCID 14868519, compound

Participants

Reaction Steps

A suspension of 2,3-bis(ethoxalylamino)benzo[b]thiophene (5.47 g, 15 mmol) in 250 ml of 4 N hydrochloric acid was heated to reflux for 2 h. Then the mixture was cooled on an ice bath, and filtered. The crude product was washed with water and recrystallized from a mixture of ethanol, DMF and water with decolorizing charcoal. The recrystallized solid was filtered off, washed with ethanol and ether, and dried for 1 h at 100° C. to give 2.2 g (62%) of the pure title compound as a monohydrate; m.p. 377.6° C. DSC); 1R (KBr): 3200-2500, 1670 cm-1 ; 1H-NMR (DMSO-d6): δ 3.3 (broad s, 2H, H2O); 7.1-7.6 (m, 2H, ArH), 7.8-8.1 (m, 2H, ArH), 11.9-13.6 (broad, 2H, 2NH); MS (m/e): 218 (M+, 100%).

Provenance & Evidence