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Cesium carbonate → HCID 69009937, 화합물

HRID 2102410
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HRID 2102410 반응식
[F:1][C:2]1[CH:7]=[C:6]([S:8][CH3:9])[CH:5]=[CH:4][C:3]=1[NH2:10].C1(P(C2C=CC=CC=2)C2(P(C3C=CC=CC=3)C3C=CC=CC=3)CC=C3C(C=CC=C3)=C2C2C3C(=CC=CC=3)C=CC=2)C=CC=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+].[CH2:63]([O:65][C:66]([C:68]1[C:73](Cl)=[C:72]([CH3:75])[N:71]2[N:76]=[CH:77][CH:78]=[C:70]2[N:69]=1)=[O:67])[CH3:64]>C1(C)C=CC=CC=1.CCOC(C)=O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH2:63]([O:65][C:66]([C:68]1[C:73]([NH:10][C:3]2[CH:4]=[CH:5][C:6]([S:8][CH3:9])=[CH:7][C:2]=2[F:1])=[C:72]([CH3:75])[N:71]2[N:76]=[CH:77][CH:78]=[C:70]2[N:69]=1)=[O:67])[CH3:64]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 10796Cesium carbonateHCID 220256172-Fluoro-4-(methylsulfanyl)anilineHCID 69005522HCID 69005522, 화합물HCID 86595863(+/-)-2,2-Bis(diphenylphosphino)-1,1-binaphthyl

생성물 1

HCID 69009937HCID 69009937, 화합물

시약·촉매·용매 3

HCID 167845
palladium(II) acetate
촉매
HCID 1140Toluene용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

2-Fluoro-4-methylsulfanyl-phenylamine (1.01 equivalents), palladium(II) acetate (0.10 equivalents), rac-2,2-bis(diphenylphosphino)-1,1′-binaphthyl (0.15 equivalents), and cesium carbonate (1.50 equivalents) are added to a solution of 6-chloro-7-methylpyrazolo[1,5-a]pyrimidine-5-carboxylic acid ethyl ester (1.00 equivalent) in toluene in a sealed vial. After stirring 10 minutes, the mixture is heated to 80° C. After 24 hours, the reaction mixture is cooled to room temperature and diluted with EtOAc. The resulting precipitate is filtered and washed with EtOAc. The filtrate is diluted with EtOAc and washed with water. The aqueous layer is re-extracted with EtOAc. The combined organic layers are washed with brine, dried (MgSO4) and concentrated. The product is purified by flash chromatography as necessary.

후처리

  1. waitAfter 24 hours
  2. temperaturethe reaction mixture is cooled to room temperature
  3. filtrationThe resulting precipitate is filtered
  4. washwashed with EtOAc
  5. additionThe filtrate is diluted with EtOAc
  6. washwashed with water
  7. extractionThe aqueous layer is re-extracted with EtOAc
  8. washThe combined organic layers are washed with brine
  9. dry with materialdried (MgSO4)
  10. concentrationconcentrated
  11. customThe product is purified by flash chromatography as necessary

출처 및 근거

ORD 기록
ord-4249cf1c88a745d69eb36390fbdb178a
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07576072B2

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