反応 #2186219

反応方程式

5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylthio-1H-pyrazole-3-carboxylic acid

dioxane

ammonia

→

title compound

収率 98.0%

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

収率 98.0%

溶媒

water

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate/heptane (1:1)
2. 2
   洗浄The combined organic phase was washed with aqueous potassium hydrogensulfate (5%)
3. 3
   乾燥dried over magnesium sulfate
4. 4
   その他evaporated

実験手順

A mixture of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylthio-1H-pyrazole-3-carboxylic acid (1.00 g, 2.27 mmol) and 1,1-dicarbonylimidazole (0.45 g, 2.72 mmol) in dioxane was heated to 50° C. for 2 hours. An aqueous solution of ammonia (33%, 80 ml) was then added and stirring continued at 50° C. for 4 hours. The cooled mixture was diluted with water and extracted with ethyl acetate/heptane (1:1). The combined organic phase was washed with aqueous potassium hydrogensulfate (5%), dried over magnesium sulfate and evaporated to give the title compound (0.980 g, yield 98%) as a white foam, 1H NMR (CDCl3): 4.36 (bs, 2H, NH2), 5.60 and 6.69 (bs, 2H, C(O)NH2), and 7.82 (s, 2H, Ar—H).

出典