Cesium carbonate → 4,4'-(4-Bromo-6-nitro-1,3-phenylene)bis(oxy)bis(1,3-difluorobenzene)

HRID 633525ノート

反応式

HRID 633525 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[C:5](F)=[CH:4][C:3]=1F.[C:13](=[O:16])([O-])[O-].[Cs+].[Cs+].[F:19][C:20]1[CH:25]=[C:24]([F:26])[CH:23]=[CH:22][C:21]=1[OH:27]>CS(C)=O>[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[C:5]([O:27][C:21]2[CH:22]=[CH:23][C:24]([F:26])=[CH:25][C:20]=2[F:19])=[CH:4][C:3]=1[O:16][C:13]1[CH:22]=[CH:21][C:20]([F:19])=[CH:25][C:24]=1[F:26]

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 1230512,4-DifluorophenolHCID 2230781-Bromo-2,4-difluoro-5-nitrobenzene

生成物 1

HCID 904167304,4'-(4-Bromo-6-nitro-1,3-phenylene)bis(oxy)bis(1,3-difluorobenzene)収率 120.1%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

To a solution of 1-bromo-2,4-difluoro-5-nitrobenzene (0.3 g, 1.26 mmol) and cesium carbonate (0.86 g, 2.65 mmol) in DMSO (6.3 mL) was added dropwise 2,4-difluorophenol (0.27 g, 2.10 mmol). The mix was stirred for 60 minutes at ambient temperature and partitioned between ethyl acetate and water, adjusting the pH to 6 with HCl. The organic layer was washed with water, saturated aqueous sodium chloride, dried (MgSO4), filtered, and concentrated to afford the title compound (0.578 g, 100%).

後処理

  1. custompartitioned between ethyl acetate and water
  2. washThe organic layer was washed with water, saturated aqueous sodium chloride
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-cfed1b56bb364f88bf20d91a422f550b
出典データセット
uspto-grants-2016_04
特許番号
US09321764B2

反応ノート

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