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

HRID 442588

반응식

HRID 442588 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

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.

후처리

  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,

출처 및 근거

ORD 기록
ord-62ba16d6b6194f72842bd59dca9816a2
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05891358

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