Potassium Iodide → [1,1'-Biphenyl]-4-carbonitrile, 4'-(decyloxy)-

HRID 442588

反応式

HRID 442588 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)=[CH:5][CH:4]=1)#[N:2].Br[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CC(=O)CC>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:11][CH:10]=2)=[CH:7][CH:8]=1)#[N:2]

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 81731-BromodecaneHCID 11430Potassium CarbonateHCID 1406104'-Hydroxy-4-biphenylcarbonitrile

生成物 1

HCID 112405[1,1'-Biphenyl]-4-carbonitrile, 4'-(decyloxy)-

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 4-cyano-4'-hydroxybiphenyl (56) (10.10 g, 0.052 mol), 1-bromodecane (14.38 g, 0.065 mol), anhydrous potassium carbonate (37.32 g, 0.27 mol), butanone (300 ml) and a trace of potassium iodide was heated under reflux overnight. The cooled solution was filtered to remove inorganic salts and the solvent was removed in vacuo. The residual oil was distilled (to remove excess bromide) and finally purified by column chromatography (dichloromethane) to yield a colourless, low melting solid.

後処理

  1. temperatureunder reflux overnight
  2. filtrationThe cooled solution was filtered
  3. customto remove inorganic salts
  4. customthe solvent was removed in vacuo
  5. distillationThe residual oil was distilled
  6. custom(to remove excess bromide)
  7. customfinally purified by column chromatography (dichloromethane)
  8. customto yield a colourless,

出典と根拠

ORDレコード
ord-62ba16d6b6194f72842bd59dca9816a2
出典データセット
uspto-grants-1999_04
特許番号
US05891358

関連ノート

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