2-Methylbiphenyl → HCID 178429793, 화합물

HRID 649696

반응식

HRID 649696 반응식
[Cl:1]C1C(C)=C(C2C=CC=CC=2)C=CC=1.[Mg:15].[CH3:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>O1CCCC1>[CH3:16][C:17]1[C:22]([Mg:15][Cl:1])=[CH:21][CH:20]=[CH:19][C:18]=1[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

참가 물질

5

반응물 3

HCID 125632-MethylbiphenylHCID 46018323-Chloro-2-methylbiphenyl2회HCID 5462224Magnesium2회

생성물 1

HCID 178429793HCID 178429793, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Under a nitrogen atmosphere, 101.3 g (0.50 mole) of 3-chloro-2-methylbiphenyl (92% purity) in 75 g of dry tetrahydrofuran was added dropwise over two hours with stirring to a gently refluxing mixture of 13.1 g (0.54 mole) of fresh magnesium turnings, the heel from a previous run containing 0.21 mole of unreacted magnesium, and 75 g of dry tetrahydrofuran in a dry reaction vessel. Upon complete addition, the reaction mixture was heated at reflux for five additional hours. Gas chromatographic analysis of a quenched sample of the reaction mixture showed 1.2% of unreacted 3-chloro-2-methylbiphenyl and 92.4% of 2-methylbiphenyl. The reaction mixture was allowed to cool overnight.

후처리

  1. temperaturea gently refluxing
  2. customin a dry reaction vessel
  3. additionUpon complete addition
  4. temperaturethe reaction mixture was heated
  5. temperatureat reflux for five additional hours
  6. temperatureto cool overnight

출처 및 근거

ORD 기록
ord-0ba85c39d27e423fa554840dca9f5c9f
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04740637

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