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HCID 57799869, 화합물 → HCID 57799540, 화합물

HRID 2101096
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HRID 2101096 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH2:13][CH2:14][C:15]([OH:17])=O)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][O:11][CH3:12]>O=S(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]2[C:5](=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][O:11][CH3:12])[C:15](=[O:17])[CH2:14][CH2:13]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 57799869HCID 57799869, 화합물

생성물 1

HCID 57799540HCID 57799540, 화합물

시약·촉매·용매 1

HCID 24386Thionyl Chloride용매

반응 조건

온도
45 °C

실험 절차

The mixture of 3-[3-Fluoro-4-(2-methoxy-ethoxy)-phenyl]-propionic acid (16 g) in SOCl2 (50 ml) was refluxed for 4 hours. The mixture was evaporated, the residue was dissolved in CS2 (100 ml), and then AlCl3 (20 g) was added. The mixture was heated at 45° C. for 4 hours. 200 ml of ice-water was added to the cooled mixture and the mixture was stirred for another 1 hour. The mixture was extracted by ethyl acetate (300 ml×3). The product was purified by flash column chromatography using ethyl acetate:PE=5:1 as eluent. LC-MS: m/e 225 (MH+).

후처리

  1. temperature
이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트
was refluxed for 4 hours
  • customThe mixture was evaporated
  • dissolutionthe residue was dissolved in CS2 (100 ml)
  • additionAlCl3 (20 g) was added
  • addition200 ml of ice-water was added to the cooled mixture
  • extractionThe mixture was extracted by ethyl acetate (300 ml×3)
  • customThe product was purified by flash column chromatography
  • 출처 및 근거

    ORD 기록
    ord-a715b30c0787431882890d2d03bc11cb
    출처 데이터셋
    uspto-grants-2009_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07572809B2

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