Acetic Acid → HCID 19834631, Verbindung

HRID 2051065Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2051065
[H][H].O.C(O)(=O)C.[N+:8]([C:11]1[C:12]([O:24][CH2:25][CH3:26])=[C:13]([Cl:23])[CH:14]=[C:15]([N+:20]([O-])=O)[C:16]=1[O:17][CH2:18][CH3:19])([O-])=O>[Fe].C(OCC)(=O)C>[ClH:23].[CH2:25]([O:24][C:12]1[C:11]([NH2:8])=[C:16]([O:17][CH2:18][CH3:19])[C:15]([NH2:20])=[CH:14][C:13]=1[Cl:23])[CH3:26]

Komponenten

7

Edukt 4

HCID 176Acetic AcidHCID 962WaterHCID 19751981HCID 19751981, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 19834631HCID 19834631, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysator2×HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

170 g of powdered iron which had been reduced with hydrogen were added to 450 ml of water containing 8.5 ml of acetic acid which have previously been heated to 80° C., and then 0.3 mole (87 g) of 3,5-dinitro-2,4-diethoxychlorobenzene was then gradually added with stirring. Upon completion of the additions, the reaction mixture was maintained in a boiling water bath for 30 additional minutes. After cooling, the reaction mixture was centrifuged. The iron slurries were made to a paste again with ethyl acetate and the mother liquors were extracted with ethyl acetate. The ethyl acetate phases, joined together, were washed with water and then dried over Na2SO4. Upon addition of a hydrochloric acid solution in ethanol, the expected product precipitated. After thorough draining, it was washed with acetone. It was recrystallized from an aqueous-alcoholic solution of hydrochloric acid.

Aufarbeitung

  1. temperatureUpon completion of the additions, the reaction mixture was maintained in a boiling water bath for 30 additional minutes
  2. temperatureAfter cooling
  3. extractionthe mother liquors were extracted with ethyl acetate
  4. washwere washed with water
  5. dry with materialdried over Na2SO4
  6. additionUpon addition of a hydrochloric acid solution in ethanol
  7. customthe expected product precipitated
  8. washAfter thorough draining, it was washed with acetone
  9. customIt was recrystallized from an aqueous-alcoholic solution of hydrochloric acid

Quellen und Nachweise

ORD-Eintrag
ord-30f90d2f6a594ebaba6159219d607982
Quelldatensatz
uspto-grants-1991_05
Patentnummer
US05015772

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