Reaktion #170174
ord-95f30f31f97f486aa7cdaaeb3b3284b4
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling down to room temperature
- 2TemperaturThe reaction mixture was again heated up to 70° C.
- 3workup.STIRRINGstirred for an additional 1.5 hours
- 4EinengenAfter concentration to dryness
- 5Sonstigethe crude mixture was triturated in pentane (2×5 mL)
Vorschrift
1-Chloroethyl chloroformate (180 μL, 1.6 mmol) was added to a solution of 1-benzhydryl-3-butoxyazetidine (370 mg, 1.2 mmol) in 1,2-dichloroethane (6 mL) at room temperature. The reaction mixture was then heated up to 70° C. and stirred for 1.5 hours. After cooling down to room temperature, methanol (7 mL) was added. The reaction mixture was again heated up to 70° C. and stirred for an additional 1.5 hours. After concentration to dryness, the crude mixture was triturated in pentane (2×5 mL) to give a yellow oil (179 mg, 86%) which was used in the next step without further purification.