تفاعل #66950

معادلة التفاعل

1H-pyrazol-3-amine

NaHCO3

Acetic anhydride

→

title compound

المردود 49.3%

N-1H-pyrazol-3-ylacetamide

المردود 49.3%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe resulting suspension was heated
2. 2
   درجة الحرارةat reflux overnight
3. 3
   أخرىthe solid obtained
4. 4
   ترشيحwas filtered off

الإجراء التجريبي

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+).

المصدر