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HCID 86747858, 화합물 → HCID 67798175, 화합물

HRID 1077957
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HRID 1077957 반응식
[C:1]1([CH2:7][O:8][C:9](=[O:49])[C@@H:10]([CH3:48])[NH:11][C:12](=[O:47])[C@@H:13]([CH2:22][CH2:23][CH2:24][CH:25]([C:37]([O:39][CH2:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)=[O:38])[NH:26][C:27]([O:29][CH2:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[O:28])[NH:14]C(OC(C)(C)C)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>C(O)(C(F)(F)F)=O>[C:1]1([CH2:7][O:8][C:9](=[O:49])[C@@H:10]([CH3:48])[NH:11][C:12](=[O:47])[C@@H:13]([CH2:22][CH2:23][CH2:24][CH:25]([C:37]([O:39][CH2:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)=[O:38])[NH:26][C:27]([O:29][CH2:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[O:28])[NH2:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 86747858HCID 86747858, 화합물

생성물 1

HCID 67798175HCID 67798175, 화합물수율 105.6%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of 40b (251 mg, 0.37 mmol) in TFA (870 μl) is stirred for 30 min at 0° C. The TFA is removed and the oil is taken up in EtOAc and washed with saturated NaHCO3 solution. Drying and removal of the solvent gives 3b (225 mg, slight excess) which is used in subsequent reactions without further handling: NMR δ 1.39 (d, 3 H) and 1.20-1.70 (overlapping m, 4 H), 1.82 (br s, 2 H), 3.23 (br s, variable, 2 H), 3.33 (br s, 1 H), 4.39 (m, 1 H), 4.47 (apparent quintet, 1 H), 5.03-5.13 (m, 6 H), 5.27 (br d, 1 H), 7.35 (m, 15 H), 7.95 (br d, 1 H); MS (FAB) m/z 576 (M+H), 598 (M+Na).

후처리

  • customThe TFA is removed
  • washwashed with saturated NaHCO3 solution
  • customDrying
  • customremoval of the solvent
  • 출처 및 근거

    ORD 기록
    ord-031ad47552b34cc39add3dc228a56a11
    출처 데이터셋
    uspto-grants-1996_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05545662

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