반응 #2186225

반응 방정식

1-(2,6-dichloro-4-trifluoromethylpheny)-5-ethoxy-4-trifluoromethylthio-1 H-pyrazole-3-carbonitrile

sulfuric acid

→

title compound

수율 73.0%

1-(2,6-Dichloro-4-trifluoromethylphenyl)-5-ethoxy-4-trifluoromethylthio-1H-pyrazole-3-carboxylic acid amide

수율 73.0%

반응 조건

후처리

1. 1
   여과the precipitate filtered off
2. 2
   세척washed with water
3. 3
   기타air-dried
4. 4
   workup.DISSOLUTIONThe crude product was dissolved in heptanes/ethyl acetate (1:1)
5. 5
   여과filtered
6. 6
   기타The filtrate was evaporated

실험 절차

A stirred mixture of 1-(2,6-dichloro-4-trifluoromethylpheny)-5-ethoxy-4-trifluoromethylthio-1 H-pyrazole-3-carbonitrile (0.55 g, 1.22 mmol) and concentrated sulfuric acid (0.55 ml) was heated at 100° C. for 3 hours. The cooled mixture was added to ice water and the precipitate filtered off, washed with water and air-dried. The crude product was dissolved in heptanes/ethyl acetate (1:1) and filtered. The filtrate was evaporated to give the title compound (0.42 g, yield 73%) as yellowish crystals, mp 161° C., 1H NMR (CDCl3): 1.32 (t, 3H, CH3), 4.68 (q, 2H, OCH2), 5.54 and 6.69 (bs, 2H, C(O)NH2), and 7.77 (s, 2H, Ar—H).

출처