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Dimethylformamide → HCID 178474488, 화합물

HRID 2205818
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인쇄 미리보기

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HRID 2205818 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:12](I)=[C:11]([NH:14][C:15](=[O:17])[CH3:16])[NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.[C:18]1([C:24]#[CH:25])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(N(CC)CC)C.CN(C=O)C>C(OCC)(=O)C.O.[Cu](I)I.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:12]([C:25]#[C:24][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[C:11]([NH:14][C:15](=[O:17])[CH3:16])[NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 10821PhenylacetyleneHCID 178474489HCID 178474489, 화합물

생성물 1

HCID 178474488HCID 178474488, 화합물수율 28.5%

시약·촉매·용매 4

HCID 83717Copper iodide촉매
HCID 178418476
HCID 178418476, 화합물
촉매
HCID 962Water용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
90 °C

실험 절차

Nitrogen was bubbled through a mixture of N-[3-(3-fluorophenyl)-4-iodo-1H-pyrazol-5-yl]acetamide (10.8 g, 44 mmol), phenyl acetylene (12.5 g, 123 mmol), triethylamine (100 mL) and DMF (40 mL) for 15 min. Copper iodide (840 mg, 4.42 mmol) and bis(triphenylphosphine)palladium(II) dichloride (1.5 g, 2.1 mmol) were added and the reaction mixture was stirred at 90° C. under nitrogen for 6 h. The reaction mixture was cooled to room temperature, diluted with ethyl acetate and water. The organic phase was washed with water and brine, dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by column chromatography (silica gel, isohexane/ethyl acetate 1:0 to 0:1) yielding the title compound as a solid (4 g).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. washThe organic phase was washed with water and brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by column chromatography (silica gel, isohexane/ethyl acetate 1:0 to 0:1)

출처 및 근거

ORD 기록
ord-69e722a36ae0477d8194ecba5b512faf
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09371332B2

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