Reaktion #721068
ord-590b7d12837c40bea8e83e4d76df40e8
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling to room temperature
- 2workup.STIRRINGthe reaction mixture was stirred at 70° C. for 1.5 h
- 3EinengenThe reaction mixture was concentrated to dryness
- 4SonstigeThe crude mixture was triturated in pentane
- 5Sonstigeto give a dark wax (140 mg, quantitative) which
- 6Sonstigewas used without further purification
Vorschrift
A 50 mL flask was charged with 1-(diphenylmethyl)-3-(2-thienylmethoxy)azetidine (204 mg, 0.61 mmol; which may be prepared as described in Step 2) and 1,2-dichloroethane (2.7 mL). 1-Chloroethyl chloroformate (86 μL, 0.79 mmol) was added and the reaction mixture was stirred at 70° C. for 1.5 h. After cooling to room temperature, methanol (2.7 mL) was added and the reaction mixture was stirred at 70° C. for 1.5 h. The reaction mixture was concentrated to dryness. The crude mixture was triturated in pentane to give a dark wax (140 mg, quantitative) which was used without further purification.