Nitric Acid → HCID 14366181, compound

Participants

Reaction Steps

40 ml of concentrated sulphuric acid are cooled to 8° C. and 5 g of the compound of Stage 1 are added while stirring. At 5° C., 5 ml of concentrated nitric acid are then added dropwise and stirring is continued for 1 hour. Subsequently the mixture is poured on 300 to 400 g of ice and the precipitated crystals are isolated by filtering with suction 4 g of a yellow crystalline compound are obtained. On recrystallizing from ethanol this compound melts at 193° C. 1H-NMR Spectrum: 10.38 (s, NH), 9.72 (s, NH), 8.23 (d, J=9 Hz, 4-H), 8.10 (d, J=9 Hz, 3-H), 4.19d (q, J=7 Hz, OCH2), 4.13 (q, J=7 Hz, OCH2), 1.25 (t, J=7 Hz, CH3), 1.23 (t, J=7 Hz, CH3)

Provenance & Evidence