Reaktion #48544
ord-9930678f962847d1aa3e1e730e0a3dbf
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturcooled to between 10 and 15° C
- 2Einengenconcentrated under reduced pressure
- 3workup.ADDITIONThe residue was diluted with ether
- 4Waschenthe solution washed with 1N hydrochloric acid, sodium carbonate solution (×3) and brine
- 5TrocknenIt was then dried over MgSO4
- 6Sonstigeevaporated under reduced pressure
Vorschrift
A solution of ethyl isonipecotate (27.6 g, 175 mmol) in dichloromethane (50 ml) was added dropwise over 10 minutes to a solution of 3-chlorobenzoyl chloride (20 ml, 160 mmol) and triethylamine (28 ml, 200 mmol) in dichloromethane (500 ml) cooled to between 10 and 15° C. The reaction was then stirred at room temperature for 3 hours and concentrated under reduced pressure. The residue was diluted with ether, the solution washed with 1N hydrochloric acid, sodium carbonate solution (×3) and brine. It was then dried over MgSO4 and evaporated under reduced pressure, to give the title compound as a solid, 44.49.