Azobisisobutyronitrile → Methyl 4'-(bromomethyl)biphenyl-2-carboxylate

HRID 53437

반응식

HRID 53437 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:17]=[CH:16][CH:15]=[CH:14][C:9]=2[C:10]([O:12][CH3:13])=[O:11])=[CH:4][CH:3]=1.[Br:18]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl.N(C(C)(C)C#N)=NC(C)(C)C#N>[Br:18][CH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:17]=[CH:16][CH:15]=[CH:14][C:9]=2[C:10]([O:12][CH3:13])=[O:11])=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 1393873(1,1'-Biphenyl)-2-carboxylic acid, 4'-methyl-, methyl ester

생성물 1

HCID 11012181Methyl 4'-(bromomethyl)biphenyl-2-carboxylate수율 59.6%

시약·촉매·용매 2

HCID 6547Azobisisobutyronitrile촉매HCID 5943Carbon Tetrachloride용매

실험 절차

2.0 g (8.8 mmol) of methyl 2-(4'-methylphenyl)benzoate, 1.6 g (9.0 mmol) of N-bromosuccinimide and 0.05 g of α,α'-azobis(isobutyronitrile) [another name; 2,2'-azobis(isobutyronitrile)] were dissolved in carbon tetrachloride (110 ml), followed by heating under reflux for 2 hours. The resultant mixture was filtered to remove insolubles, and then vacuum concentration was effected. The residue was recrystallized from a n-hexane/isopropyl ether mixed solvent to give 1.6 g of the title compound (yield; 59%).

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 2 hours
  3. filtrationThe resultant mixture was filtered
  4. customto remove insolubles
  5. concentrationvacuum concentration
  6. customThe residue was recrystallized from a n-hexane/isopropyl ether mixed solvent

출처 및 근거

ORD 기록
ord-11522c2bf8264c559cda5831527097e2
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05618969

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