Reaktion #721081

ord-2b207a3abcef40249eefd6e166628ab1

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
    TemperaturThe reaction mixture was cooled
  4. 4
    Einengenconcentrated to dryness
  5. 5
    SonstigeThe 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%).

Quelle

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