4,4'-Dichloro-3,3'-dinitrobenzophenone → 3,3'-Diaminobenzophenone

HRID 637547

反応式

HRID 637547 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:19]=[CH:20][C:21]=1Cl)[C:7]([C:9]1[CH:14]=[CH:13][C:12](Cl)=[C:11]([N+:16]([O-])=O)[CH:10]=1)=[O:8])([O-])=O.[O-2].[Ca+2].[H][H]>[Pd].ClCCCl>[NH2:1][C:4]1[CH:5]=[C:6]([CH:19]=[CH:20][CH:21]=1)[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([NH2:16])[CH:10]=1)=[O:8]

参加物

6

反応物 3

HCID 3483014,4'-Dichloro-3,3'-dinitrobenzophenoneHCID 6850728CalciumoxideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 691453,3'-Diaminobenzophenone

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 111,2-Dichloroethane溶媒

反応条件

温度
70 °C

実験手順

To an autoclave there are added 50 g (0.15 moles) of 3,3'-dinitro-4,4'-dichloro benzophenone, 21 g (0.38 moles) of calcium oxide, 1 g of 5% palladium/alumina catalyst (available from Nihon-Engelhardt Co., Ltd.) and 350 ml of 1,2-dichloro ethane. The reaction is carried out for ten hours by introducing hydrogen into the autoclave, with the mixture being stirred at 30°-35° C., to keep the pressure at 10 Kg/cm2.G. After the completion of the reaction, the reaction mixture is heated up to 70° C. and subjected to a hot filtering so as to remove the catalyst and the inorganic salt. On cooling the mixture there are obtained yellow needle-like crystals of 3,3'-diamino benzophenone. The crystals are filtered, washed with 10 ml of 1,2-dichloro ethane and dried. Yield 21.2 g (67%). M.P. 149°-150.5° C. Recrystallization from ethanol gives pure crystals. M.P. 150°-151° C.

後処理

  1. waitThe reaction is carried out for ten hours
  2. customAfter the completion of the reaction
  3. filtrationa hot filtering so as
  4. customto remove the catalyst
  5. temperatureOn cooling the mixture there

出典と根拠

ORDレコード
ord-320100a0c75c4b7296d3cb6866d9835d
出典データセット
uspto-grants-1985_12
特許番号
US04556738

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