Sodium Carbonate → HCID 57264076、化合物

HRID 539254

反応式

HRID 539254 の反応式
[CH3:1][O:2][C:3]1[C:8]([O:9][CH3:10])=[CH:7][CH:6]=[CH:5][C:4]=1B(O)O.[F:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1Br.C(=O)([O-])[O-].[Na+].[Na+]>COCCOC>[F:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[C:4]1[CH:5]=[CH:6][CH:7]=[C:8]([O:9][CH3:10])[C:3]=1[O:2][CH3:1]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 612591-Bromo-2-fluorobenzeneHCID 51564912,3-Dimethoxybenzeneboronic acid

生成物 1

HCID 57264076HCID 57264076、化合物収率 85%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

In the atmosphere of argon, 18.2 g of 2,3-dimethoxyphenylboronic acid, 17.5 g of 2-fluorobromobenzene, 2.31 g of tetrakistriphenylphosphine palladium (0), 300 mL of 1,2-dimethoxyethane and 150 mL of an aqueous 2M sodium carbonate solution were placed in a flask. The resulting mixture was stirred with heating under reflux for 8 hours. After cooling to room temperature, an aqueous phase was removed, and an organic phase was washed with saturated saline. The organic phase was dried with magnesium sulfate and then concentrated. Residues were purified by silica gel column chromatography, whereby 19.7 g of (yield 85%) of 2′-fluoro-2,3-dimethoxybiphenyl was obtained.

後処理

  1. temperaturewith heating
  2. temperatureunder reflux for 8 hours
  3. customan aqueous phase was removed
  4. washan organic phase was washed with saturated saline
  5. dry with materialThe organic phase was dried with magnesium sulfate
  6. concentrationconcentrated
  7. customResidues were purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-61096a40444346a482859d4c2af2deb3
出典データセット
uspto-grants-2014_10
特許番号
US08866135B2

関連ノート

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