반응 #1583820

반응 방정식

5-methyl-1-[2,2,2-trifluoro-1-(trifluoromethyl)ethyl]pyrazole-4-carbonyl chloride

pyridazin-4-amine

triethylamine

→

title compound

수율 90.0%

5-methyl-1-(2,2,2-trifluoro-1-trifluoromethyl-ethyl)-1H-pyrazole-4-carboxylic acid pyridazin-4-ylamide

수율 90.0%

용매

CH2Cl2

CH2Cl2

ethylacetate

반응 조건

후처리

1. 1
   세척washed with 3×15 ml sat. aq. NH4Cl solution
2. 2
   건조dried over MgSO4
3. 3
   기타evaporated
4. 4
   기타Purification by flash chromatography (CH2Cl2/MeOH)

실험 절차

A solution of 398 mg 5-methyl-1-[2,2,2-trifluoro-1-(trifluoromethyl)ethyl]pyrazole-4-carbonyl chloride in 10 ml CH2Cl2 was added dropwise to a solution of 185 mg pyridazin-4-amine and 750 mg triethylamine in 30 ml CH2Cl2 at 0° C. The mixture was stirred at 20-25° C. for about 68 h, diluted with 25 ml ethylacetate, washed with 3×15 ml sat. aq. NH4Cl solution, dried over MgSO4 and evaporated. Purification by flash chromatography (CH2Cl2/MeOH) gave 160 mg of the title compound (90% purity). HPLC-MS (Method 1): RT 2.278 min, m/z [MH]+ 354.1.

출처