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

HRID 637547

반응식

HRID 637547 반응식
[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]

참가 물질

6

반응물 3

HCID 3483014,4'-Dichloro-3,3'-dinitrobenzophenoneHCID 6850728CalciumoxideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 691453,3'-Diaminobenzophenone

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 111,2-Dichloroethane용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-320100a0c75c4b7296d3cb6866d9835d
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04556738

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