HCID 86686569, 화합물 → 4'-Fluorospiro[cyclobutane-1,3'-indol]-2'(1'H)-one

HRID 1528090노트

반응식

HRID 1528090 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([N+:8]([O-])=O)[C:3]=1[C:11]1([C:15]([O:17]C)=O)[CH2:14][CH2:13][CH2:12]1>C(O)(=O)C.[Zn]>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]2[C:3]=1[C:11]1([CH2:14][CH2:13][CH2:12]1)[C:15](=[O:17])[NH:8]2

참가 물질

4

반응물 1

HCID 86686569HCID 86686569, 화합물

생성물 1

HCID 866865714'-Fluorospiro[cyclobutane-1,3'-indol]-2'(1'H)-one수율 97.9%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

실험 절차

To a solution of methyl 1-(2-fluoro-6-nitrophenyl)cyclobutanecarboxylate (3.11 g) in acetic acid (60 mL) was added zinc (16.1 g), and the mixture was stirred overnight at room temperature. The zinc was removed by filtration, and the filtrate was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate. The solution was washed with saturated aqueous sodium hydrogen carbonate solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.30 g).

후처리

  1. customThe zinc was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washThe solution was washed with saturated aqueous sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-583c37fc649c4e0593a695c600aec3d2
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09090586B2

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