Chloral → HCID 13341913, compound

Participants

Reaction Steps

5-Nitroanthranilamide (6.5 g.) and anhydrous chloral (65 ml.) were stirred together at ambient temperature, until thin layer chromatography indicated that all the 5-nitroanthranilamide had disappeared (6 days). The excess of chloral was distilled off, and the resulting syrup was heated with concentrated sulphuric acid (125 ml.) on a steam bath for 10 minutes. The reaction mixture was cooled and poured into ice/water (1 kg.), and the solid product which was precipitated was filtered off, washed with water (3×200 ml.) and crystallised from ethanol (450 ml.) to give 1,2-dihydro-6-nitro-2-trichloromethylquinazolin-4-one, m.p. 278°-280° C.

Provenance & Evidence