Réaction #60588

ord-9f3bad2d120440b88a6b4d3df793da91

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    ConcentrationThe reaction mixture was concentrated under reduced pressure
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in methanol (10 ml)
  3. 3
    TempératureThe solution was refluxed for 1 h
  4. 4
    Concentrationconcentrated under reduced pressure
  5. 5
    AutreThe crude product was crystallized from ethyl acetate
  6. 6
    Filtrationfiltrated

Mode opératoire

A solution of 2-benzoyl-4-benzylmorpholine (600 mg, 2.13 mmol) and chloroformic acid 1-chloromethyl ester (457 mg, 3.20 mmol) in 1,2-dichloroethane (8.0 ml) was refluxed for 1 h. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in methanol (10 ml). The solution was refluxed for 1 h and concentrated under reduced pressure. The crude product was crystallized from ethyl acetate and filtrated to give 2-benzoylmorpholine hydrochloride (323 mg, 67%) as a colorless crystal.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07427615B2uspto-grants-2008_09