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Potassium Carbonate → Ethyl 5-bromo-2-(2-nitropyridin-3-yl)-3-oxo-2,3-dihydro-1-benzofuran-2-carboxylate

HRID 931376
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HRID 931376 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][CH:8]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:7](=[O:15])[C:6]=2[CH:16]=1.[N+:17]([C:20]1[C:25](F)=[CH:24][CH:23]=[CH:22][N:21]=1)([O-:19])=[O:18].C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([C:25]3[C:20]([N+:17]([O-:19])=[O:18])=[N:21][CH:22]=[CH:23][CH:24]=3)([C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:7](=[O:15])[C:6]=2[CH:16]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 27628023-Fluoro-2-nitropyridineHCID 58458886Ethyl 5-bromo-3-oxo-2,3-dihydro-1-benzofuran-2-carboxylate

생성물 1

HCID 58458882Ethyl 5-bromo-2-(2-nitropyridin-3-yl)-3-oxo-2,3-dihydro-1-benzofuran-2-carboxylate

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
87.5 °C

실험 절차

A mixture of ethyl 5-bromo-3-oxo-2,3-dihydro-1-benzofuran-2-carboxylate (1.42 g, 5.0 mmol), 2-nitro-3-fluoropyridine (0.71 g, 5 mmol) and potassium carbonate (0.83 g, 6.0 mmol) in DMSO (15 mL) is heated at 85-90° C. for 18 h. The mixture is cooled to ambient temperature and partitioned between EtOAc and brine. The layers are separated and the aqueous layer is further extracted with EtOAc. The combined organic extracts are dried (Na2SO4), filtered and concentrated in vacuo. The residue is purified by silica gel chromatography (gradient elution with hexanes-EtOAc) to afford the title compound.

후처리

  1. temperatureThe mixture is cooled to ambient temperature
  2. custompartitioned between EtOAc and brine
  3. customThe layers are separated
  4. extractionthe aqueous layer is further extracted with EtOAc
  5. dry with materialThe combined organic extracts are dried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue is purified by silica gel chromatography (gradient elution with hexanes-EtOAc)

출처 및 근거

ORD 기록
ord-3e8ea1c00e014b29a6944455a9b9c773
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296750B2

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