Acetic Acid → Mls000756290

HRID 461296

Reaktionsgleichung

Reaktionsgleichung von HRID 461296
[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].C(O)(=O)C>[Ni]>[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 3

HCID 176Acetic AcidHCID 7918Acetic AnhydrideHCID 37089224-Ethylamino-3-nitrobenzamide

Produkt 1

HCID 292579Mls000756290Ausbeute 88 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 935NickelKatalysator

Versuchsvorschrift

A mixture of 125 g (0.6 mole) of compound III, 214 g (2.1 moles) of acetic anhydride, 1.2 ml of Raney nickel and 36 g (0.6 mole) of acetic acid was hydrogenated at 80° C and a pressure of 100 to 30 kg/sq.cm for 5 h. After cooling, the catalyst was filtered, and the filtrate was concentrated by normal pressure until 135 ml of distillate were collected. Then 150 ml of 6N sulphuric acid 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 sodium hydroxide. The precipitate was washed with water and dried at 100° C. Melting point: 251° C. Yield: 88% (108 g).

Aufarbeitung

  1. customwas hydrogenated at 80° C
  2. temperatureAfter cooling
  3. filtrationthe catalyst was filtered
  4. concentrationthe filtrate was concentrated by normal pressure until 135 ml of distillate
  5. customwere collected
  6. additionThen 150 ml of 6N sulphuric acid were added to the residue
  7. temperatureThe solution was refluxed with active carbon for 15 min
  8. filtrationfiltered
  9. additionThe filtrate was mixed with 1.2 kg of ice
  10. washThe precipitate was washed with water
  11. customdried at 100° C

Quellen und Nachweise

ORD-Eintrag
ord-8053dfd953ee47138cdbee4d00589cb3
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04062682

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