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Thionyl Chloride → HCID 19783302, 화합물

HRID 257476
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반응식

HRID 257476 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH:9](O)[CH:10]([C:12]1[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=1)[CH3:11].S(Cl)(Cl)=O>>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8]/[CH:9]=[C:10](\[C:12]1[CH:13]=[CH:14][N:15]=[CH:16][CH:17]=1)/[CH3:11]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24386Thionyl ChlorideHCID 19783305HCID 19783305, 화합물

생성물 1

HCID 19783302HCID 19783302, 화합물수율 36.6%

반응 조건

온도
40 °C

실험 절차

To the said solid, that is, 1.59 g (6.49 mmol) of 1-(2-fluorophenyl)-3-(4-pyridyl)-2-butanol, 2.5 ml of thionyl chloride was added and stirred for one hour at 40° C. After distilling away excessive thionyl chloride under reduced pressure, water was added and the residue was alkalized with sodium carbonate and was extracted with ethyl acetate. After drying over anhydrous sodium sulfate, ethyl acetate was distilled away under reduced pressure to obtain a brown oily substance. The resulting oily substance was purified by silica gel column chromatography to obtain 0.54 g of the desired compound (yield: 31.6%).

후처리

distillation
After distilling away excessive thionyl chloride under reduced pressure, water
  • additionwas added
  • extractionwas extracted with ethyl acetate
  • dry with materialAfter drying over anhydrous sodium sulfate, ethyl acetate
  • distillationwas distilled away under reduced pressure
  • customto obtain a brown oily substance
  • customThe resulting oily substance was purified by silica gel column chromatography
  • 출처 및 근거

    ORD 기록
    ord-1d5fe70ccd91474db0ddf7bfd8c7a36f
    출처 데이터셋
    uspto-grants-1993_11
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05262420

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