Reaktion #2259220

ord-47656b198f414038afa9dbfa211a07ca

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstige1 hour
  2. 2
    Sonstigeat 70° C
  3. 3
    TemperaturAfter cooling down to room temperature
  4. 4
    workup.STIRRINGthe reaction mixture was stirred at 70° C. for 1 hour
  5. 5
    EinengenAfter concentration to dryness
  6. 6
    Sonstigethe crude mixture was triturated in pentane (2×15 mL)
  7. 7
    Sonstigeto give a yellow oil (698 mg, quantitative) which
  8. 8
    Sonstigewas used in the next step without further purification

Vorschrift

1-Chloroethylchloroformate (361 μL, 3.33 mmol) was added to a solution of 1-benzhydryl-3-(2-(thiophen-2-yl)ethoxy)azetidine (1.11 g, 3.17 mmol) in dichloromethane (15 mL) at room temperature. The reaction mixture was stirred overnight at room temperature, then 1 hour at 70° C. After cooling down to room temperature, ethanol (15 mL) was added and the reaction mixture was stirred at 70° C. for 1 hour. After concentration to dryness, the crude mixture was triturated in pentane (2×15 mL) to give a yellow oil (698 mg, quantitative) which was used in the next step without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09051321B2uspto-grants-2015_06