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

HRID 651310

反応式

HRID 651310 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-32777e1a215a4a0dac166d894cb7b24c
出典データセット
uspto-grants-2001_08
特許番号
US06278028B1

関連ノート

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