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99113-85-6 → HCID 67268960, 화합물

HRID 251740
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HRID 251740 반응식
[C:1]1([C:7]2[CH:8]=[C:9]([CH:12]=[O:13])[O:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>C1COCC1>[C:1]1([C:7]2[CH:8]=[C:9]([CH:12]([OH:13])[CH2:12][CH2:9][CH2:8][CH2:7][CH2:1][CH:2]=[CH2:3])[O:10][CH:11]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

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HCID 1354168999113-85-6

생성물 1

HCID 67268960HCID 67268960, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The resulting Grignard solution was added to a solution of 4-phenyl-2-furaldehyde (1 eq.) in THF at 0° C. under Ar and the mixture was stirred for 30 min. The reaction was quenched by slow addition of sat. aq. NH4Cl solution and the desired product was extracted with EtOAc. The organic layer was washed with brine, dried (Na2SO4) and concentrated under reduced pressure. The crude was purified by column chromatography eluting with 5% EtOAc/Petroleum ether to afford the desired alcohol. 1H NMR (300 MHz, CD3Cl3) δ: 7.65 (2H, d, J=7.3 Hz), 7.42 (2H, t, J=7.2 Hz), 7.25-7.15 (1H, m), 6.60 (1H, d, J=5.3 Hz), 6.30 (1H, d, J=5.3 Hz), 5.87-5.75 (1H, m), 5.05-4.89 (2H, m), 4.75-4.65 (1H, m), 2.15-2.05 (2H, m), 1.87-1.75 (2H, m), 1.45-1.35 (6H, m). MS (ES) C18H22O2 requires: 270 found: 271 (M+H)+.

후처리

  1. custom
The reaction was quenched by slow addition of sat. aq. NH4Cl solution
  • extractionthe desired product was extracted with EtOAc
  • washThe organic layer was washed with brine
  • dry with materialdried (Na2SO4)
  • concentrationconcentrated under reduced pressure
  • customThe crude was purified by column chromatography
  • washeluting with 5% EtOAc/Petroleum ether
  • 출처 및 근거

    ORD 기록
    ord-9176b2c73d3448aa83c9a842f7ed39fb
    출처 데이터셋
    uspto-grants-2011_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07863294B2

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