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Phosphorus oxychloride → HCID 59511172, 화합물

HRID 1157823
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HRID 1157823 반응식
[C:1]([N:9]1[CH2:14][CH2:13][N:12]([C:15]2[C:20]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[N:19][NH:18][C:17](=O)[CH:16]=2)[CH2:11][CH2:10]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:30])=O>>[Cl:30][C:17]1[N:18]=[N:19][C:20]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[C:15]([N:12]2[CH2:13][CH2:14][N:9]([C:1]([C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)=[O:8])[CH2:10][CH2:11]2)[CH:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 14909614HCID 14909614, 화합물

생성물 1

HCID 59511172HCID 59511172, 화합물

반응 조건

온도
80 °C

실험 절차

To 5-(4-benzoylpiperazin-1-yl)-6-phenylpyridazin-3(2H)-one (1.3 g) taken in single necked round bottom flask, phosphorusoxychloride (10 ml) was added and the mixture was heated to 80° C. for 4 hrs. Reaction mixture was cooled to room temperature and concentrated to remove excess phosphorus oxychloride. Residue was slowly poured into ice and neutralized with solid sodium bicarbonate. The mixture was extracted with Ethyl acetate (3×100 ml). The combined organic layer was dried over anhydrous sodium sulphate and concentrated to afford (4-(6-chloro-3-phenylpyridazin-4-yl)piperazin-1-yl)(phenyl)methanone as white solid.

후처리

  1. custom
Reaction mixture
  • temperaturewas cooled to room temperature
  • concentrationconcentrated
  • customto remove excess phosphorus oxychloride
  • additionResidue was slowly poured into ice and neutralized with solid sodium bicarbonate
  • extractionThe mixture was extracted with Ethyl acetate (3×100 ml)
  • dry with materialThe combined organic layer was dried over anhydrous sodium sulphate
  • concentrationconcentrated
  • 출처 및 근거

    ORD 기록
    ord-aeee1f2299424a08bb407737cad75383
    출처 데이터셋
    uspto-grants-2010_10
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07807676B2

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