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Methanol → HCID 46203371, 화합물

HRID 524159
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HRID 524159 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[C:15]([CH3:17])([CH3:16])[C:14](=[O:18])[N:13]([CH:19]3[CH2:24][CH2:23][N:22]([S:25]([C:28]4[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=4)[C:31]([OH:33])=[O:32])(=[O:27])=[O:26])[CH2:21][CH2:20]3)[N:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].S(=O)(=O)(O)O.[CH3:42]O>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[C:15]([CH3:17])([CH3:16])[C:14](=[O:18])[N:13]([CH:19]3[CH2:24][CH2:23][N:22]([S:25]([C:28]4[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=4)[C:31]([O:33][CH3:42])=[O:32])(=[O:26])=[O:27])[CH2:21][CH2:20]3)[N:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 46203370HCID 46203370, 화합물

생성물 1

HCID 46203371HCID 46203371, 화합물

실험 절차

0.5 g 3-({4-[3-(3,4-Dimethoxyphenyl)-4,4-dimethyl-5-oxo-4,5-dihydro-1H-pyrazol-1-yl]piperidin-1-yl}sulfonyl)benzoic acid (compound described in example 25) are suspended in 20 ml of methanol, 0.2 ml concentrated sulfuric acid are added, and the reaction mixture is heated to reflux for 24 h. The solvent is removed under reduced pressure, the residue is taken up in DCM, the organic phase is washed with aqueous sodium carbonate solution (5%) and dried over MgSO4. The solvents are evaporated under reduced pressure and the crude product is crystallized from DCM and diethyl ether to yield the title compound.

후처리

  • temperaturethe reaction mixture is heated
  • temperatureto reflux for 24 h
  • customThe solvent is removed under reduced pressure
  • washthe organic phase is washed with aqueous sodium carbonate solution (5%)
  • dry with materialdried over MgSO4
  • customThe solvents are evaporated under reduced pressure
  • customthe crude product is crystallized from DCM and diethyl ether
  • 출처 및 근거

    ORD 기록
    ord-f6b04691e31a4210880a67c856662400
    출처 데이터셋
    uspto-grants-2016_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US09340522B2

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