Реакция #163123

Уравнение реакции

2,5,6-trifluoronicotinonitrile

triethylamine

5-isopropoxy-1H-pyrazol-3-amine

→

title compound

Выход 9.0%

2,5-Difluoro-6-(5-isopropoxy-1H-pyrazol-3-ylamino)nicotinonitrile

Выход 9.0%

Растворители

water

ACN

ACN

Условия реакции

Обработка

1. 1
   Экстракцияextracted with DCM (2×50 ml)
2. 2
   СушкаThe combined organic fractions were dried over Na2SO4
3. 3
   Фильтрацияfiltered
4. 4
   Концентрированиеconcentrated
5. 5
   ДругоеThe resulting oil was purified by column chromatography (DCM-MeOH=100:1)

Методика

To a solution of 2,5,6-trifluoronicotinonitrile (3.0 g, 19.0 mmol) and triethylamine (2.5 g, 24.7 mmol) in ACN (30 ml) at 0° C. was added 5-isopropoxy-1H-pyrazol-3-amine (2.95 g, 20.9 mmol) in ACN (15 ml). The reaction was stirred at 0° C. for 1 hour, at which point the reaction was diluted with water (50 ml) and extracted with DCM (2×50 ml). The combined organic fractions were dried over Na2SO4, filtered, and then concentrated. The resulting oil was purified by column chromatography (DCM-MeOH=100:1) to give the title compound (0.48 g, 9%). MS: Calcd.: 279. Found: [M+H]+ 280.

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