Ammonia → Ethyl acetate hexane

HRID 443033

Reaktionsgleichung

Reaktionsgleichung von HRID 443033
[OH:1][C:2]1[C:15]2[C:6](=CC3C(N=2)=CC=CC=3)[CH:5]=[CH:4][CH:3]=1.C(C(CCCC)CN(CC(CC)CCCC)C1C=CC(N)=CC=1)C.[CH2:40]([OH:42])[CH3:41].N>O.[N+]([O-])([O-])=O.[Ag+]>[CH3:6][CH2:15][CH2:2][CH2:3][CH2:4][CH3:5].[C:40]([O:1][CH2:2][CH3:15])(=[O:42])[CH3:41]

Komponenten

7

Edukt 4

HCID 222AmmoniaHCID 702EthanolHCID 874624-HydroxyacridineHCID 53999179n,n-Di(2-ethylhexyl)-p-phenylenediamine

Produkt 1

HCID 21226206Ethyl acetate hexaneAusbeute 12,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24470Silver NitrateKatalysatorHCID 962WaterLösungsmittel2×

Versuchsvorschrift

While stirring a mixture comprising 2.87 g of 4-hydroxyacridine (20), 4.89 g of N,N-di(2-ethylhexyl)-p-phenylenediamine and 100 ml of ethanol at 20° C., a solution comprising 7.48 g of silver nitrate dissolved in 33.1 ml of water was added thereto drop-by-drop. Next, with 12.5 ml of 25% ammonia solution added to the mixture, reaction was allowed to proceed at 20° C. for a period of 24 hr. After the completion of the reaction, the reacted solution was introduced into water. After extraction by ethyl acetate, the extract was concentrated. After purification by column chromatography, 0.99 g of indoaniline described in the exemplified compound 4-10 was obtained as deep blue crystals on recrystallization by hexane-ethyl acetate (yield 12.9%).

Aufarbeitung

  1. additionwas added
  2. customAfter the completion of the reaction
  3. extractionAfter extraction by ethyl acetate
  4. concentrationthe extract was concentrated
  5. customAfter purification by column chromatography, 0.99 g of indoaniline

Quellen und Nachweise

ORD-Eintrag
ord-fd39022622144649972d930330e7c148
Quelldatensatz
uspto-grants-1999_04
Patentnummer
US05892042

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