Reaktion #4392
ord-022e022fa6a34c4ca3ba0dec5c804a5d
Reaktionsgleichung
2-amino-3-(2-methylbenzylamino)pyridine
chloroacetone
→
8-(2-methylbenzylamino)-2-methylimidazo[1,2-a]pyridine
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigeevaporated in vacuo
- 2workup.ADDITIONTo the residue was added aqueous sodium bicarbonate solution
- 3Extraktionthe mixture was extracted with methylene chloride
- 4WaschenThe extract was washed with brine
- 5Trocknendried over magnesium sulfate
- 6Sonstigeevaporated in vacuo
- 7SonstigeThe oily residue was purified by column chromatography on silica gel (40 g) with a mixture of methylene chloride and ethyl acetate (10:1) as an eluent
Vorschrift
A solution of 2-amino-3-(2-methylbenzylamino)pyridine (3.25 g) and chloroacetone (1.26 ml) in ethanol (65 ml) was refluxed for 18 hours and then evaporated in vacuo. To the residue was added aqueous sodium bicarbonate solution and the mixture was extracted with methylene chloride. The extract was washed with brine, dried over magnesium sulfate, and evaporated in vacuo. The oily residue was purified by column chromatography on silica gel (40 g) with a mixture of methylene chloride and ethyl acetate (10:1) as an eluent to give 8-(2-methylbenzylamino)-2-methylimidazo[1,2-a]pyridine (1.80 g).