Ammonia → Ethyl acetate hexane

HRID 581211

Reaktionsgleichung

Reaktionsgleichung von HRID 581211
[OH:1][C:2]1[C:15]2[C:6](=C3C(=CN=2)C=CC=C3)[CH:5]=[CH:4][CH:3]=1.Cl.NC1C=CC(N(CC)CC)=CC=1C.[CH2:30]([OH:32])[CH3:31].N>O.[N+]([O-])([O-])=O.[Ag+]>[CH3:6][CH2:15][CH2:2][CH2:3][CH2:4][CH3:5].[C:30]([O:1][CH2:2][CH3:15])(=[O:32])[CH3:31]

Komponenten

7

Edukt 4

HCID 222AmmoniaHCID 702EthanolHCID 108623N,N-Diethyltoluene-2,5-diamine hydrochlorideHCID 22625105Phenanthridin-4-ol

Produkt 1

HCID 21226206Ethyl acetate hexaneAusbeute 35,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24470Silver NitrateKatalysatorHCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

A mixture comprising 390 mg of 4-hydroxyphenanthridine (13), 430 mg of 2-amino-5-diethylaminotoluene hydrochloride (21) and 15 ml of ethanol was stirred at 20° C. and a solution comprising 1.02 g of silver nitrate dissolved in 4.5 ml of water was added thereto drop-by-drop. Then, 1.7 ml of 25% ammonia solution was added and the 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, 259 mg of deep blue crystal of indoaniline (22) was obtained on recrystallization by hexane-ethyl acetate (yield 35.1%).

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, 259 mg of deep blue crystal of indoaniline (22)

Quellen und Nachweise

ORD-Eintrag
ord-32b02fce559647e8bdf3b75b797f3c03
Quelldatensatz
uspto-grants-1999_07
Patentnummer
US05919928

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