반응 #1583821

반응 방정식

5-methyl-1-[2,2,2-trifluoro-1-(trifluoromethyl)ethyl]pyrazole-4-carboxylic acid

N-methylpyridazin-4-amine

O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate

triethylamine

→

title compound

수율 90.0%

N,5-dimethyl-N-pyridazin-4-yl-1-[2,2,2-trifluoro-1-(trifluoromethyl)ethyl]pyrazole-4-carboxamide

수율 90.0%

용매

THF

반응 조건

후처리

1. 1
   기타evaporated
2. 2
   세척washed with 3×14 ml water
3. 3
   건조dried over Na2SO4
4. 4
   기타evaporated
5. 5
   기타Purification by flash chromatography (CH2Cl2/MeOH)

실험 절차

A mixture of 300 mg 5-methyl-1-[2,2,2-trifluoro-1-(trifluoromethyl)ethyl]pyrazole-4-carboxylic acid, 127 mg N-methylpyridazin-4-amine, 710 mg O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate [HATU] and 220 mg triethylamine in 30 ml THF was stirred at 20-25° C. for about 24 h, then evaporated. The residue was taken up in 21 ml CH2Cl2, washed with 3×14 ml water, dried over Na2SO4, then evaporated. Purification by flash chromatography (CH2Cl2/MeOH) gave 130 mg of the title compound (90% purity).

출처