Reaktion #46975
ord-3196d557fb8848f3bf1af18536d3e07f
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturto reflux for 15 h
- 2TemperaturAfter cooling
- 3Sonstigethe reaction mixture was evaporated
- 4Extraktionextracted by CH2Cl2
- 5TrocknenThe combined organic layer was dried by MgSO4
- 6Einengenconcentrated
- 7Sonstigeto give a residue that
- 8Sonstigewas purified by silica gel flash column chromatography (EtOAc:n-hexane=1:2)
Vorschrift
To a stirred solution of 18 (2 g, 4.84 mmol), AIBN (0.08 g, 0.48 mmol), Bu3SnH (3.91 ml, 14.50 mmol) in toluene (49 ml) was heated to reflux for 15 h. After cooling, the reaction mixture was evaporated and then extracted by CH2Cl2. The combined organic layer was dried by MgSO4 and concentrated to give a residue that was purified by silica gel flash column chromatography (EtOAc:n-hexane=1:2) to give compound 19, yield 90%.