Реакция #2186219

Уравнение реакции

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

dioxane

ammonia

→

title compound

Выход 98.0%

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

Выход 98.0%

Растворители

water

Условия реакции

Обработка

1. 1
   Экстракцияextracted with ethyl acetate/heptane (1:1)
2. 2
   ПромывкаThe combined organic phase was washed with aqueous potassium hydrogensulfate (5%)
3. 3
   Сушкаdried over magnesium sulfate
4. 4
   Другоеevaporated

Методика

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).

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