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

HRID 985354

反応式

HRID 985354 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2659042974c14e1aae337a3b51e2e52d
出典データセット
uspto-grants-2005_03
特許番号
US06870978B2

関連ノート

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