Reaktionsgleichung
C[O:2][C:3]1[C:4]([N+:13]([O-])=O)=[CH:5][C:6]([N+:10]([O-])=O)=[C:7]([OH:9])[CH:8]=1.[ClH:16]>[Pd].O>[ClH:16].[ClH:16].[NH2:10][C:6]1[CH:5]=[C:4]([NH2:13])[C:3]([OH:2])=[CH:8][C:7]=1[OH:9]Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 55 °C
Versuchsvorschrift
A 500 mL, 3-necked, round-bottomed flask is charged with 150 mL of water, 21.4 g (0.1 mole) of 5-methoxy-2,4-dinitrophenol and 1.0 g of 10% palladium on carbon catalyst. The reaction is stirred under a nitrogen atmosphere for 3 to 4 minutes. The stirred reaction mixture is heated to 55° C. and hydrogen gas is sparged below the surface of the reaction mixture. After 10 minutes, 19.8 g (0.2 mole) of concentrated HCl is added through the condenser while hydrogenation is continued for 4 hours. The catalyst is removed by filtration and the filtrate is passed into a solution consisting of 0.5 g of stannous chloride dihydrate and 25 mL of concentrated HCl. This solution is then saturated with dry HCl gas and charged to a 600 mL 5 Hastalloy B autoclave. The reactor is heated to 150° C. for 18 hours and cooled to 25° C. The resulting product is isolated by filtration and dried under nitrogen to yield 19.7 g (90% yield) of crude 4,6-diaminoresorcinol dihydrochloride.
Aufarbeitung
- customThe stirred reaction mixture
- customhydrogen gas is sparged below the surface of the reaction mixture
- waitAfter 10 minutes
- waitis continued for 4 hours
- customThe catalyst is removed by filtration
- additionsaturated with dry HCl gas and charged to a 600 mL 5 Hastalloy B autoclave
- temperatureThe reactor is heated to 150° C. for 18 hours
- temperaturecooled to 25° C
- customThe resulting product is isolated by filtration
- customdried under nitrogen
Quellen und Nachweise
- ORD-Eintrag
- ord-9362d9d8bb4f40b3b1cd41825c183e44
- Quelldatensatz
- uspto-grants-1995_05
- Patentnummer
- US05414130
Verknüpfte Notizen
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