Reaktion #721081
ord-2b207a3abcef40249eefd6e166628ab1
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
- 3TemperaturThe reaction mixture was cooled
- 4Einengenconcentrated to dryness
- 5SonstigeThe residue was purified on column chromatography (eluent: Pentane/NH3 7N in MeOH, 98/2)
Vorschrift
A 16 mL vial was charged with 3-(benzyloxy)-1-(diphenylmethyl)azetidine (103 mg, 0.31 mmol; which may be prepared as described in Step 1) and 1,2-dichloroethane (1.4 mL). 1-Chloroethyl chloroformate (45 μL, 0.41 mmol) was added and the reaction mixture was stirred at 70° C. for 1.5 h. After cooling to room temperature, methanol (1.4 mL) was added and the reaction mixture was stirred at 70° C. for 1.5 h. The reaction mixture was cooled and concentrated to dryness. The residue was purified on column chromatography (eluent: Pentane/NH3 7N in MeOH, 98/2) to give the title compound (57 mg, 92%).