Acetic Anhydride → HCID 178474341, compound

Participants

Reaction Steps

1H-pyrazol-3-amine (ALDRICH, 11.32 g, 0.136 mol) was dissolved in 100 mL of distilled water. NaHCO3 (34 g, 0.408 mol) was slowly added. Acetic anhydride (27.55 g, 0.272 mol) was then added dropwise and the resulting suspension was heated at reflux overnight. Then, the mixture was allowed to cool down to r.t. and the solid obtained was filtered off and characterized as the title compound (8.4 g, 0.067 mol, 49%). After concentration of the filtrate, a second precipitate was obtained (2.7 g, 0.021 mol, 16%), also characterized as the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm: 12.23 (br s, 1H), 10.30 (br s, 1H), 7.55 (br s, 1H), 6.45 (br s, 1H), 1.97 (s, 3H). [ES+MS] m/z 126 (MH+).

Provenance & Evidence