반응 #66950

반응 방정식

1H-pyrazol-3-amine

NaHCO3

Acetic anhydride

→

title compound

수율 49.3%

N-1H-pyrazol-3-ylacetamide

수율 49.3%

용매

water

반응 조건

후처리

1. 1
   온도the resulting suspension was heated
2. 2
   온도at reflux overnight
3. 3
   기타the solid obtained
4. 4
   여과was filtered off

실험 절차

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+).

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