Reaktion #44097

ord-8292b4c04b144d2f893018d610388da4

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenThe mixture was washed with a saturated solution of ammonium chloride (2×3 vol)
  2. 2
    EinengenThe organic phase was concentrated to 5 vol, ethyl acetate (5 vol)
  3. 3
    workup.ADDITIONwas added
  4. 4
    Sonstigethe solution was evaporated to dryness

Vorschrift

Alternatively, 1-[3-(2-hydroxyethyl)phenyl]-2-imidazolidinone was suspended in acetonitrile (5 vol) at room temperature and under nitrogen. Triethylamine (1 vol) was added dropwise over 15 minutes. The mixture was cooled to 0° C. and methanesulfonyl chloride (0.73 vol) was added over 30 minutes. The reaction mixture was stirred at room temperature for 2 hours, then diluted with ethyl acetate (10 vol). The mixture was washed with a saturated solution of ammonium chloride (2×3 vol), followed by water-brine 1:1 (2×3 vol). The organic phase was concentrated to 5 vol, ethyl acetate (5 vol) was added and the solution was evaporated to dryness, yielding the title compound as a cream-coloured solid (yield: 90% th).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732600B2uspto-grants-2010_06