Sodium Carbonate → 3,3'-Diaminobenzophenone

HRID 637557Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 637557
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]

Komponenten

6

Edukt 3

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

Produkt 1

HCID 691453,3'-Diaminobenzophenone

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-427fbe334cca4260af1426e7f16c5a62
Quelldatensatz
uspto-grants-1985_12
Patentnummer
US04556738

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