Réaction #2322432

ord-f749f7325e60485eb2f92e116bc354f3

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrethe reaction at room temperature for 24 hours until the starting material
  2. 2
    ExtractionAdd saturated NaHCO3 (100 mL) and extract the aqueous layer with ethyl acetate (3×200 mL)
  3. 3
    SéchageCombine the organic layers and dry with Na2SO4
  4. 4
    Filtrationfilter
  5. 5
    Concentrationconcentrate

Mode opératoire

Dissolve 3-(2,4-dichloro-benzyl)-1-(cis-7-methyl-1,4-dioxa-spiro[4.5]dec-8-yl)-pyrrolidin-2-one (2.34 g, 5.87 mmol) in acetone (100 mL) and add TsOH (1.01 g, 5.87 mmol). Stir the reaction at room temperature for 24 hours until the starting material has been gone. Add saturated NaHCO3 (100 mL) and extract the aqueous layer with ethyl acetate (3×200 mL). Combine the organic layers and dry with Na2SO4, filter and concentrate to give 1.95 g (94%) of the crude title compound as a white solid: Mass spectrum (ion spray): m/z=354.2, 356.1 (M+1).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07713979B2uspto-grants-2010_05