Reaktion #721068

ord-590b7d12837c40bea8e83e4d76df40e8

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling to room temperature
  2. 2
    workup.STIRRINGthe reaction mixture was stirred at 70° C. for 1.5 h
  3. 3
    EinengenThe reaction mixture was concentrated to dryness
  4. 4
    SonstigeThe crude mixture was triturated in pentane
  5. 5
    Sonstigeto give a dark wax (140 mg, quantitative) which
  6. 6
    Sonstigewas 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09321769B2uspto-grants-2016_04