Reaktionsgleichung
[C:1]1([N:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH:9]=[CH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:16][C:17]([NH2:19])=[S:18].[I-:20].[K+].II>CO.C(O)C.O>[IH:20].[C:1]1([N:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9]([S:18][C:17](=[NH:16])[NH2:19])=[CH:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Versuchsvorschrift
N-Phenylindole (28.95 g; 0.15M) and thiourea (11.4 g; 0.15M) were dissolved in a mixture of methanol (140 ml) and ethanol (100 ml) by rapid stirring at 20°. To this solution was added in four portions a solution of potassium iodide (52.5 g; 0.3M) and iodine (38.1 g; 0.15M) in water (60 ml) over 10 minutes. The solution was then stirred at 20° for 17 hours. The resulting heavy yellow precipitate of the crude product was filtered off, washed successively with isopropanol (3×200 ml), water (3×200 ml), isopropanol (3×200 ml) and ether (2×200 ml), and then dried at 60° to give the title compound, weight 46.2 g (78.0% yield). An analytical sample was prepared by crystallisation from a 1:1 mixture of methanol and ethanol. This gave colourless rhombohedral crystals of the title compound, m.p. 264°-6°.
Aufarbeitung
- stirringThe solution was then stirred at 20° for 17 hours
- filtrationThe resulting heavy yellow precipitate of the crude product was filtered off
- washwashed successively with isopropanol (3×200 ml), water (3×200 ml), isopropanol (3×200 ml) and ether (2×200 ml)
- customdried at 60°
Quellen und Nachweise
- ORD-Eintrag
- ord-41317134c12548ee83cb47f889119cc6
- Quelldatensatz
- uspto-grants-1985_12
- Patentnummer
- US04558048
Verknüpfte Notizen
Wird geladen…