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Ethyl orthoformate → HCID 136337142, 화합물

HRID 519659
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HRID 519659 반응식
[CH2:1]([C:5]1[N:6]=[C:7]([NH:27][NH2:28])[NH:8][C:9](=[O:26])[C:10]=1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[C:19]([C:24]#[N:25])=[CH:20][CH:21]=[CH:22][CH:23]=2)=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH3:4].[CH:29](OCC)(OCC)OCC>>[CH2:1]([C:5]1[N:6]2[CH:29]=[N:28][N:27]=[C:7]2[NH:8][C:9](=[O:26])[C:10]=1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[C:19]([C:24]#[N:25])=[CH:20][CH:21]=[CH:22][CH:23]=2)=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 31214Ethyl orthoformateHCID 136337141HCID 136337141, 화합물

생성물 1

HCID 136337142HCID 136337142, 화합물수율 17%

반응 조건

온도
100 °C

실험 절차

A mixture of 4′-[(4-butyl-2-hydrazino-6-oxo-1,6-dihydropyrimidin-5-yl)methyl]biphenyl-2-carbonitrile (2.6 g) and triethyl orthoformate (30 mL) was stirred at 100° C. for 16 hr. The reaction mixture was concentrated, and ethyl acetate and water were added to the obtained residue. The ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound as a colorless solid (0.46 g, 17%).

후처리

  • concentrationThe reaction mixture was concentrated
  • additionethyl acetate and water were added to the obtained residue
  • washThe ethyl acetate layer was washed with saturated brine
  • dry with materialdried over anhydrous magnesium sulfate
  • customThe solvent was evaporated under reduced pressure
  • customThe obtained residue was purified by silica gel column chromatography
  • 출처 및 근거

    ORD 기록
    ord-483fd2a0b5b74ff8ac34226d35cd90f7
    출처 데이터셋
    uspto-grants-2015_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US09115136B2

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