2,2'-Bis(trifluoromethyl)-4,4'-dinitrobiphenyl → (1,1'-Biphenyl)-4,4'-diamine, 2,2'-bis(trifluoromethyl)-

HRID 985354

반응식

HRID 985354 반응식
[F:1][C:2]([F:26])([F:25])[C:3]1[CH:8]=[C:7]([N+:9]([O-])=O)[CH:6]=[CH:5][C:4]=1[C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-])=O)=[CH:14][C:13]=1[C:21]([F:24])([F:23])[F:22]>[Pd].C(OCC)(=O)C>[F:1][C:2]([F:25])([F:26])[C:3]1[CH:8]=[C:7]([NH2:9])[CH:6]=[CH:5][C:4]=1[C:12]1[CH:17]=[CH:16][C:15]([NH2:18])=[CH:14][C:13]=1[C:21]([F:22])([F:23])[F:24]

참가 물질

4

반응물 1

HCID 113724052,2'-Bis(trifluoromethyl)-4,4'-dinitrobiphenyl

생성물 1

HCID 629349(1,1'-Biphenyl)-4,4'-diamine, 2,2'-bis(trifluoromethyl)-수율 90%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

A hydrogenation bottle was charged with 40.0 g of 2,2′-bis(trifluoromethyl)-4,4′-dinitrobiphenyl, 0.6 g of 5% palladium on activated carbon and 200 ml of ethyl acetate. The bottle was secured on a Parr hydrogenation apparatus, flushed five times with hydrogen, and then pressurized with hydrogen to 56 psi. The pressure was maintained, and the vessel was agitated for several hours. After the reaction mixture was filtered and about 200 ml of hexanes were added. The crystals that formed were filtered to afford 30.2 g (90%) of product.

후처리

  1. customflushed five times with hydrogen
  2. temperatureThe pressure was maintained
  3. filtrationAfter the reaction mixture was filtered
  4. additionabout 200 ml of hexanes were added
  5. customThe crystals that formed
  6. filtrationwere filtered

출처 및 근거

ORD 기록
ord-2659042974c14e1aae337a3b51e2e52d
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06870978B2

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