Reaktion #67281

ord-17a5df4cda5c49fea3146204156f6994

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenthe resulting mixture was washed with HCl (1 N) and brine
  2. 2
    TrocknenThe organic phase was dried (Na2SO4)
  3. 3
    Sonstigeevaporated to dryness

Vorschrift

A solution of [5-fluoro-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methanol (0.4 g, 1.7 mmol), toluenesulfonyl chloride (0.5 g, 2.6 mmol), TEA (0.4 ml, 2.6 mmol) and 4-DMAP (0.2 g, 1.7 mmol) in DCM (10 ml) was stirred at rt for 1 h. DCM was added and the resulting mixture was washed with HCl (1 N) and brine. The organic phase was dried (Na2SO4) and evaporated to dryness to give the title compound (0.7 g). MS m/z (rel. intensity, 70 eV) 416 (M+, 31), 244 (bp), 243 (26), 231 (19), 91 (70).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524766B2uspto-grants-2013_09