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

HRID 83488

반응식

HRID 83488 반응식
[C:1]1([N:7]2[CH:11]=[CH:10][C:9]([NH2:12])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:13][C:14](=O)[CH2:15][CH2:16][C:17](=O)[CH3:18]>C(O)(=O)C>[CH3:18][C:17]1[N:12]([C:9]2[CH:10]=[CH:11][N:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[N:8]=2)[C:14]([CH3:13])=[CH:15][CH:16]=1

참가 물질

4

반응물 2

HCID 80352,5-HexanedioneHCID 5943201-phenyl-1H-pyrazol-3-amine

생성물 1

HCID 712878563-(2,5-Dimethylpyrrol-1-yl)-1-phenyl-1H-pyrazole

시약·촉매·용매 1

HCID 176Acetic Acid용매

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).

후처리

  1. temperatureat reflux
  2. concentrationacetic acid was concentrated under reduced pressure
  3. additiontoluene (100 ml) was added
  4. concentrationthe mixture was further concentrated
  5. customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate 100/1 to 20/1)

출처 및 근거

ORD 기록
ord-d6cc9c75209b44ca98adb1e56a69c812
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846746B2

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