Reaktion #721128

ord-4e8ceae1c37745c795b13652c57703e7

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    TemperaturAfter cooling down to room temperature
  2. 2
    workup.STIRRINGthe reaction mixture was stirred overnight at 70° C
  3. 3
    EinengenThe mixture was then concentrated to dryness
  4. 4
    Sonstigethe residue was triturated in pentane (2×15 mL)

Vorschrift

1-Chloroethyl chloroformate (102 μL, 0.9 mmol) was added to a solution of 1-benzhydryl-3-(2-methoxyethoxy)-azetidine (215 mg, 0.7 mmol) in 1,2-dichloroethane (3 mL) at room temperature. The reaction mixture was then heated up to 70° C. and stirred for 2.5 hours. After cooling down to room temperature, methanol (3 mL) was added and the reaction mixture was stirred overnight at 70° C. The mixture was then concentrated to dryness and the residue was triturated in pentane (2×15 mL) to give a yellow oil (109 mg, 90%) which was used in the next step without further purification.

Quelle

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