Hydrochloric Acid → HCID 67199988, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of A5 in 1,4-dioxane (20 mL) was added 1.5 M aq HCl (5 mL) and the reaction mixture was refluxed for 2 h. The reaction mixture was then diluted with MeOH/EtOAc, brought to boil and allowed to cool to 20° C. The resulting precipitate was filtered, washed with EtOAc and dried to give essentially pure A6 as a pale yellow solid (1.20 g, 100%); mp (MeOH/EtOAc) 152-155; 1H NMR [(CD3)2SO] 14.35 (br, 1 H, N+H), 10.50 (br, 2 H, NH2), 8.27 (d, J=6.6 Hz, 1 H, ArH), 7.92 (d, J=9.4 Hz, 1 H, ArH), 7.65 (dd, J=9.5, 2.6 Hz, 1 H, ArH), 7.57 (d, J=2.4 Hz, 1 H, ArH), 7.54 (d, J=8.5 Hz, 2 H, ArH), 7.41 (d, J=8.1 Hz, 2H, ArH), 6.68 (d, J=6.7 Hz, 1 H, ArH), 3.12 (s, 6 H, [N(CH3)2]; APCI+ve 279.

Provenance & Evidence