반응 #170670

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1-phenyl-1H-pyrazol-3-ylamine

2,5-hexanedione

→

titled compound

3-(2,5-Dimethylpyrrol-1-yl)-1-phenyl-1H-pyrazole

용매

acetic acid

반응 조건

후처리

1. 1
   온도at reflux
2. 2
   농축acetic acid was concentrated under reduced pressure
3. 3
   workup.ADDITIONtoluene (100 ml) was added
4. 4
   농축the mixture was further concentrated
5. 5
   기타The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate 100/1 to 20/1)

실험 절차

To a solution of 1-phenyl-1H-pyrazol-3-ylamine (32.7 g) in acetic acid (330 ml) was added 2,5-hexanedione (25 ml), and the mixture was stirred for 3 hours at reflux. This reaction solution was cooled to room temperature, and then acetic acid was concentrated under reduced pressure, and then toluene (100 ml) was added thereto, and the mixture was further concentrated. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate 100/1 to 20/1) to give the titled compound (41.8 g).

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