Reaktion #5842
ord-98066fc44b1d4119929f1efebf1ad116
Reaktionsgleichung
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1workup.STIRRINGfurther stirred at a room temperature overnight
- 2SonstigeAfter evaporating off the pyridine under a reduced pressure
- 3Extraktionthe mixture was extracted twice with 50 ml of chloroform/isopropanol (10:1)
- 4TrocknenThe extract was dried over magnesium sulfate
- 5Sonstigeevaporated under a reduced pressure
- 6Sonstigeto remove the solvent
- 7workup.ADDITIONTo the resulting residue was added 20 ml of benzene/chloroform (3:1)
- 8Temperaturthe mixture was slightly warmed
- 9Sonstigecollected
Vorschrift
3.06 g of 3,4-dimethoxyaniline was dissolved in 30 ml of pyridine, to the solution was added in small portions 5.28 g of 5-isoquinolinesulfonyl chloride.HCl with stirring under ice cooling, and the mixture was stirred for 30 minutes, and further stirred at a room temperature overnight. After evaporating off the pyridine under a reduced pressure and additing 20 ml of water, the mixture was extracted twice with 50 ml of chloroform/isopropanol (10:1). The extract was dried over magnesium sulfate and evaporated under a reduced pressure to remove the solvent. To the resulting residue was added 20 ml of benzene/chloroform (3:1), and the mixture was slightly warmed and collected to obtain 5.64 g of the title compound as colorless crystals.