반응 #67281

ord-17a5df4cda5c49fea3146204156f6994

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척the resulting mixture was washed with HCl (1 N) and brine
  2. 2
    건조The organic phase was dried (Na2SO4)
  3. 3
    기타evaporated to dryness

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524766B2uspto-grants-2013_09