Azane;hydrate → (3-Aminophenyl)(4-aminophenyl)methanone

HRID 637552노트

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HRID 637552 반응식
Br[C:2]1[CH:18]=[CH:17][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][CH:9]=2)=[O:7])=[CH:4][C:3]=1[N+:19]([O-])=O.[H][H].O.N>[Pd].O1CCOCC1>[NH2:19][C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][CH:2]=1)[C:6]([C:8]1[CH:9]=[CH:10][C:11]([NH2:14])=[CH:12][CH:13]=1)=[O:7]

참가 물질

6

반응물 3

HCID 12896473Azane;hydrateHCID 197081834-Bromo-3,4'-dinitro benzophenoneHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 148536(3-Aminophenyl)(4-aminophenyl)methanone

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 312751,4-Dioxane용매

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온도
30 °C

실험 절차

In a closed vessel equipped with a thermometer and a stirrer there are charged 105 g (0.3 moles) of 4-bromo-3,4'-dinitro benzophenone, 5 g of 5% palladium/active carbon catalyst (from Nihon-Engelhardt Co.) and 300 ml of dioxane. At 70°-80° C., with the mixture being stirred, there is introduced 41 l (1.83 moles) of hydrogen so as to be absorbed in the mixture in about 11 hours. Following cooling the mixture to 30° C., there is added 38.5 g (0.33 moles) of 30% ammonia water. Then, again with the mixture being stirred, at 30°-40° C., there is introduced an additional amount of hydrogen, 7.2 l (0.32 moles), during seven hours. The reaction liquid is filtered at 30°-40° C. to remove the catalyst and then allowed to cool giving yellow crystals of 3,4'-diamino benzophenone. The crystals are filtered, washed with 30 ml of 50% aqueous dioxane solution and dried. Yield 58 g (91%). M.P. 121°-123° C.

후처리

  1. customIn a closed vessel equipped with a thermometer and a stirrer there
  2. customto be absorbed in the mixture in about 11 hours
  3. stirringThen, again with the mixture being stirred, at 30°-40° C.
  4. customThe reaction liquid
  5. filtrationis filtered at 30°-40° C.
  6. customto remove the catalyst
  7. temperatureto cool

출처 및 근거

ORD 기록
ord-d9d6e48ed041483793cece1ab1cd589c
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04556738

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