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Benzene → 4-Methoxy-3-fluoro-4"-cyano-p-terphenyl

HRID 36822
ノート
印刷プレビュー

反応式

HRID 36822 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([C:14]#[N:15])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].C1C=CC=CC=1.[CH3:28][O:29][C:30]1[CH:35]=[CH:34][C:33](B(O)O)=[CH:32][C:31]=1[F:39]>C(O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:28][O:29][C:30]1[CH:35]=[CH:34][C:33]([C:2]2[CH:7]=[CH:6][C:5]([C:8]3[CH:13]=[CH:12][C:11]([C:14]#[N:15])=[CH:10][CH:9]=3)=[CH:4][CH:3]=2)=[CH:32][C:31]=1[F:39]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 241BenzeneHCID 10340Sodium CarbonateHCID 13944624'-bromo-[1,1'-Biphenyl]-4-carbonitrileHCID 27821943-Fluoro-4-methoxyphenylboronic acid

生成物 1

HCID 220796294-Methoxy-3-fluoro-4"-cyano-p-terphenyl収率 88.6%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 702Ethanol溶媒

実験手順

To a mixture of 2.4 g of 4-bromo-4'-cyanobiphenyl, 0.37 g of tetrakis(triphenylphosphine)palladium(0), 15.2 ml of a 2N aqueous sodium carbonate solution, and 19.4 ml of benzene, a solution which was prepared by dissolving 1.9 g of 4-methoxy-3-fluoro-benzene boronic acid synthesized in [1] above in 14.4 ml of ethanol was slowly added dropwise with stirring, and the solution was subjected to reflux for 8 hours. After the reflux was finished, the solution was cooled, and the crystals thus precipitated were separated by filtration and washed with water and methanol in turn, and dried to obtain 2.5 g of 4-methoxy-3-fluoro-4"-cyano-p-terphenyl.

後処理

  1. customa solution which was prepared
  2. additionwas slowly added dropwise
  3. temperatureto reflux for 8 hours
  4. temperaturethe solution was cooled
  5. customthe crystals thus precipitated
  6. customwere separated by filtration
  7. washwashed with water and methanol in turn
  8. customdried

出典と根拠

ORDレコード
ord-856c078c427a48308a9a01c4b78b789f
出典データセット
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05417885

反応ノート

読み込み中…

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