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Methanol → HCID 66915353, 화합물

HRID 1931778
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HRID 1931778 반응식
[CH3:1][O-:2].[Na+].[C:4]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH:14]([N:17]2[C:21]3=[N:22][C:23](Cl)=[N:24][C:25](Cl)=[C:20]3[CH:19]=[N:18]2)[CH2:13][CH2:12]1)=[O:10])([CH3:7])([CH3:6])[CH3:5].[CH3:28][OH:29]>>[C:4]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH:14]([N:17]2[C:21]3=[N:22][C:23]([O:29][CH3:28])=[N:24][C:25]([O:2][CH3:1])=[C:20]3[CH:19]=[N:18]2)[CH2:13][CH2:12]1)=[O:10])([CH3:7])([CH3:6])[CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 57964878HCID 57964878, 화합물2회

생성물 1

HCID 66915353HCID 66915353, 화합물

실험 절차

Sodium methoxide (4 mmol) is added to a mixture of 4-(4,6-dichloro-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester (Intermediate 24; 1 mmol) in methanol. The resulting mixture is heated at reflux for 8 h and then cooled. The solvent is evaporated, and ethyl acetate and water are added. The organic layer is washed with water and brine, dried (magnesium sulfate), filtered, evaporated, and purified by flash chromatography on silica gel to give 4-(4,6-dimethoxy-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester.

후처리

  1. temperature
The resulting mixture is heated
  • temperatureat reflux for 8 h
  • temperaturecooled
  • customThe solvent is evaporated
  • additionethyl acetate and water are added
  • washThe organic layer is washed with water and brine
  • dry with materialdried (magnesium sulfate)
  • filtrationfiltered
  • customevaporated
  • custompurified by flash chromatography on silica gel
  • 출처 및 근거

    ORD 기록
    ord-41e502a1375f4766a69cc75af44e2f5c
    출처 데이터셋
    uspto-grants-2012_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08188098B2

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