반응 #66953

반응 방정식

5-methyl-1H-pyrazol-3-amine

phthalic anhydride

→

title compound

수율 79.0%

2-(5-methyl-1H-pyrazol-3-yl)-1H-isoindole-1,3(2H)-dione

수율 79.0%

용매

1,4-dioxane

반응 조건

후처리

1. 1
   온도at reflux for 25 hours
2. 2
   기타Reaction
3. 3
   기타to reach room temperature
4. 4
   여과the formed precipitate was filtered
5. 5
   세척washed with EtOH

실험 절차

In a 100 mL round-bottom flask a mixture of 5-methyl-1H-pyrazol-3-amine (Aldrich, 500 mg, 5.15 mmol) and phthalic anhydride (ALDRICH) (1.07 g, 7.21 mmol) in 1,4-dioxane (30 mL) was stirred at reflux for 25 hours. Reaction was allowed to reach room temperature and the formed precipitate was filtered and washed with EtOH to afford 589 mg of the title compound as a yellowish solid. Filtrate was evaporated to dryness and after washing the residue with EtOH, an additional batch of 331 mg was obtained (total yield: 79%). 1H NMR (300 MHz, DMSO-d6) δ ppm: 12.77 (br s, 1H), 7.87-7.98 (m, 4H), 6.09 (s, 1H), 2.28 (s, 3H). [ES+MS] m/z 228 (MH+).

출처