4'-(Bromomethyl)-2-cyanobiphenyl → 2-Cyano-4'-methylbiphenyl

HRID 443078노트

반응식

HRID 443078 반응식
Br[CH:2](Br)[C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:15]#[N:16])=[CH:5][CH:4]=1.BrCC1C=CC(C2C=CC=CC=2C#N)=CC=1>C1(C)C=CC=CC=1>[CH3:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:15]#[N:16])=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 15019124'-(Bromomethyl)-2-cyanobiphenylHCID 111002274'-(Dibromomethyl)[1,1'-biphenyl]-2-carbonitrile

생성물 1

HCID 1455122-Cyano-4'-methylbiphenyl

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

After the dropwise addition of the solution prepared by dissolving the mixture of 4'-dibromomethyl-2-cyanobiphenyl and 4'-bromomethyl-2-cyanobiphenyl in toluene was terminated, the mixture was allowed to react up to a point where the above suspension no longer absorbs hydrogen gas. After the reaction was terminated, Raney catalyst and sodium carbonate were filtered off, and the reaction mixture was then concentrated to distill off methanol and toluene. The resulting crude 4'-methyl-2-cyanobiphenyl was purified by distillation, to give 7.4 g of 4'-methyl-2-cyanobiphenyl having an LC purity of 98.2%.

후처리

  1. additionAfter the dropwise addition of the solution
  2. customprepared
  3. dissolutionby dissolving
  4. customwas terminated
  5. customto react up to a point where the above suspension no longer absorbs hydrogen gas
  6. customAfter the reaction was terminated
  7. filtrationRaney catalyst and sodium carbonate were filtered off
  8. concentrationthe reaction mixture was then concentrated
  9. distillationto distill off methanol and toluene
  10. distillationThe resulting crude 4'-methyl-2-cyanobiphenyl was purified by distillation

출처 및 근거

ORD 기록
ord-aa50b0f8aff3430c92ea45fe2186bb22
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05892094

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