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Trifluoroacetic acid → HCID 59750273, 화합물

HRID 499347
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반응식

HRID 499347 반응식
[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[S:5][C:4]([C:12]2[N:17]=[CH:16][C:15]([CH2:18][CH2:19][CH2:20][O:21][CH2:22][CH2:23][C:24]([O:26]C(C)(C)C)=[O:25])=[CH:14][CH:13]=2)=[N:3]1.FC(F)(F)C(O)=O>>[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[S:5][C:4]([C:12]2[N:17]=[CH:16][C:15]([CH2:18][CH2:19][CH2:20][O:21][CH2:22][CH2:23][C:24]([OH:26])=[O:25])=[CH:14][CH:13]=2)=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 86628980HCID 86628980, 화합물

생성물 1

HCID 59750273HCID 59750273, 화합물수율 66%

실험 절차

tert-Butyl 3-{3-[6-(4-oxo-4H-1,3-benzothiazin-2-yl)-3-pyridyl]propoxy}propanoate (1.0 g, 2.3 mmol) and trifluoroacetic acid (4.0 ml) was stirred under ice cooling condition for 5 hrs. The reaction mixture was concentrated under reduced pressure, diluted with chloroform, washed with water and dried. The solvent was evaporated. The residue was subjected to a silica gel column chromatography, eluted with ethyl acetate-methanol (20:1, v/v) and recrystallized from chloroform-ethyl acetate to give the titled compound (0.55 g, 66%).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additiondiluted with chloroform
  3. washwashed with water
  4. custom
dried
  • customThe solvent was evaporated
  • washeluted with ethyl acetate-methanol (20:1
  • customv/v) and recrystallized from chloroform-ethyl acetate
  • 출처 및 근거

    ORD 기록
    ord-cca0feae838d4238b8f581be244dfbba
    출처 데이터셋
    uspto-grants-2010_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07767665B2

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