Hydrochloric Acid → HCID 67202054, compound

Participants

Reaction Conditions

Reaction Steps

p-Aminobenzoic acid (D1) (1.48 g, 10.8 mmol) and 4-chloro-6-methyl-2-pyrimidinamine (A8) (1.60 g, 11.9 mmol) was dissolved in warm 2-ethoxyethanol (20 mL),then two drops of c.HCl was added and refluxed for 1 h. The reaction mixture was cooled to 20° C. and the resulting precipitate was filtered washed with more 2-ethoxyethanol and EtOAc. The solid was boiled in MeOH, cooled and filtered washed with more MeOH and dried to give D2 (2.89 g, 95%); m.p. (MeOH)>300° C.; 1H NMR [(CD3)2SO] δ12.93 (br, 1 H, N+H or COOH), 12.80 (br, 1 H, N+H or COOH), 10.87 (s, 1 H, NH), 7.92 (s, 6 H, ArH &NH2)), 6.27 (s, 1 H, ArH), 2.32 (s, 3 H, CH3); mass APCI+ 245.

Provenance & Evidence