Acetic Anhydride → Mls000756290

HRID 1729582

Reaktionsgleichung

Reaktionsgleichung von HRID 1729582
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[NH:13][CH2:14][CH3:15])[C:7]([NH2:9])=[O:8])([O-])=O.[C:16](OC(=O)C)(=O)[CH3:17]>[Ni].C(O)(=O)C>[CH2:14]([N:13]1[C:12]2[CH:11]=[CH:10][C:6]([C:7](=[O:8])[NH2:9])=[CH:5][C:4]=2[N:1]=[C:16]1[CH3:17])[CH3:15]

Komponenten

5

Edukt 2

HCID 7918Acetic AnhydrideHCID 37089224-Ethylamino-3-nitrobenzamide

Produkt 1

HCID 292579Mls000756290

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A mixture of III (125 g - 0.6 mole), acetic anhydride (214 g - 2.1 moles), Raney Nickel (1.2 ml) and acetic acid (36 g - 0.6 mole) was hydrogenated at 80° C and a pressure of 100 to 30 atm. Reaction time: 5 hours. After cooling, the catalyst was filtered, the filtrate was concentrated by normal pressure until 135 ml of distillate were collected. 150 ml of H2SO4 6N were added to the residue. The reaction was very exothermic. The solution was refluxed with active carbon for 15 min. and filtered. The filtrate was mixed with 1.2 kg of ice and exactly neutralized with 2N NaOH. The precipitate was washed with water and dried at 100° C.

Aufarbeitung

  1. customwas hydrogenated at 80° C
  2. customReaction time
  3. custom5 hours
  4. temperatureAfter cooling
  5. filtrationthe catalyst was filtered
  6. concentrationthe filtrate was concentrated by normal pressure until 135 ml of distillate
  7. customwere collected
  8. addition150 ml of H2SO4 6N were added to the residue
  9. temperatureThe solution was refluxed with active carbon for 15 min.
  10. filtrationfiltered
  11. additionThe filtrate was mixed with 1.2 kg of ice
  12. washThe precipitate was washed with water
  13. customdried at 100° C.

Quellen und Nachweise

ORD-Eintrag
ord-27961eb4825241f79cc2ef007d9cc5e1
Quelldatensatz
uspto-grants-1976_11
Patentnummer
US03989522

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