HCID 12295945, Verbindung → HCID 178511987, Verbindung

HRID 1612876Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1612876
[C:1]1([NH:11][C:12]#[N:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.Cl.[I:15][C:16]1[CH:28]=[CH:27][CH:26]=[CH:25][C:17]=1[NH:18]C1C=CC=CC=1>ClC1C=CC=CC=1>[C:1]1([NH:11][C:12]([NH:18][C:17]2[CH:25]=[CH:26][CH:27]=[CH:28][C:16]=2[I:15])=[NH:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 2

HCID 12295945HCID 12295945, VerbindungHCID 70061414HCID 70061414, Verbindung

Produkt 1

HCID 178511987HCID 178511987, VerbindungAusbeute 33,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7964ChlorobenzeneLösungsmittel

Versuchsvorschrift

A solution of 1-naphthylcyanamide (182 mg, 1.08 mmol) and o-iodophenylaniline hydrochloride (279 mg, 1.09 mmol) in chlorobenzene (5 ml) was heated at 135°-140° C. for 14 hours. It was concentrated and the residue was partitioned between dichloromethane and 10% NaOH solution. The organic layer was dried over Na2SO4 and concentrated. The resulting light green residue was recrystallized from 95% EtOH-H2O to give N-(1-naphthyl)-N'-(o-iodophenyl)-guanidine (140 mg, 33%) as off-white needles. mp 154°-155° C.

Aufarbeitung

  1. concentrationIt was concentrated
  2. customthe residue was partitioned between dichloromethane and 10% NaOH solution
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated
  5. customThe resulting light green residue was recrystallized from 95% EtOH-H2O

Quellen und Nachweise

ORD-Eintrag
ord-a1164a16b1774936bfcf117e444a8398
Quelldatensatz
uspto-grants-1993_03
Patentnummer
US05190976

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