Sodium Carbonate → 3,3'-Diaminobenzophenone

HRID 637557노트

반응식

HRID 637557 반응식
Cl[C:2]1[CH:19]=[CH:18][C:17]([N+:20]([O-])=O)=[CH:16][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][C:9](F)=[C:8]([N+:13]([O-])=O)[CH:7]=1)=[O:5].C(=O)([O-])[O-].[Na+].[Na+].[H][H]>[Pd].C(O)C>[NH2:13][C:8]1[CH:7]=[C:6]([CH:11]=[CH:10][CH:9]=1)[C:4]([C:3]1[CH:2]=[CH:19][CH:18]=[C:17]([NH2:20])[CH:16]=1)=[O:5]

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 202571122-Chloro-4'-fluoro-5,3'-dinitro benzophenoneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 691453,3'-Diaminobenzophenone

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

In an autoclave there are added 32.5 g (0.1 moles) of 2-chloro-4'-fluoro-5,3'-dinitro benzophenone, 15.9 g (0.15 moles) of sodium carbonate, 2 g of 5% palladium/alumina catalyst (from Nihon-Engelhardt Co.) and 100 ml of ethanol. With the mixture being stirred at 30°-35° C., there is introduced hydrogen into the autoclave, at a constant pressure of 10 Kg/cm2. G, to carry out the reaction for ten hours. After the completion of the reaction, the reaction mixture is heated up to filter out the catalyst and the inorganic salt. Then, on cooling the mixture there is obtained 3,3'-diamino benzophenone in the form of yellow needle-like crystals. The crystals are filtered, washed with 10 ml of ethanol and dried. Yield 16.2 g (76.3%). M.P. 149°-151° C.

후처리

  1. customthe reaction for ten hours
  2. customAfter the completion of the reaction
  3. temperaturethe reaction mixture is heated up
  4. filtrationto filter out the catalyst
  5. temperatureThen, on cooling the mixture there

출처 및 근거

ORD 기록
ord-427fbe334cca4260af1426e7f16c5a62
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04556738

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