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Water → 3-(4-Fluorophenyl)-5-isopropyl-1,2-diphenylpyrrole

HRID 1086818
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HRID 1086818 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH2:17][C:18](=O)[CH:19]([CH3:21])[CH3:20])[C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=O)=[CH:4][CH:3]=1.[NH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1.C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:17]=[C:18]([CH:19]([CH3:21])[CH3:20])[N:23]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[C:9]=2[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 6115AnilineHCID 143002712-(4-Fluorophenyl)-5-methyl-1-phenylhexane-1,4-dione

생성물 1

HCID 144613403-(4-Fluorophenyl)-5-isopropyl-1,2-diphenylpyrrole

시약·촉매·용매 2

HCID 1140Toluene용매
HCID 8857
Ethyl Acetate
용매

실험 절차

10.1 g (34 mmol) of 2-(4-fluorophenyl)-5-methyl-1-phenylhexane-1,4-dione (Example 2) and 9.3 g (102 mmol) of aniline are heated under reflux for 24 hours in a water separator in 150 ml of toluene with the addition of 500 mg of p-toluenesulphonic acid. After cooling and diluting with ethyl acetate, the mixture is washed with 1N hydrochloric acid and then with sodium hydrogen carbonate solution, dried over magnesium sulphate and concentrated in vacuo. The residue is then chromatographed over silica gel.

후처리

  1. temperatureAfter cooling
  2. washthe mixture is washed with 1N hydrochloric acid
  3. dry with materialwith sodium hydrogen carbonate solution, dried over magnesium sulphate
  4. concentrationconcentrated in vacuo
  5. customThe residue is then chromatographed over silica gel

출처 및 근거

ORD 기록
ord-3d712d5eca9244a8812ebc3d16afb676
출처 데이터셋
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05032590

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