반응 #67270

ord-d57b1b6bb37145008773e9440c539675

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Preparation
  2. 2
    세척The combined organic phases were washed with LiCl (5%, 100 ml), HCl (1 N, 100 ml), brine (100 ml)
  3. 3
    기타were evaporated to dryness
  4. 4
    기타The residue was purified by flash column chromatography (isooctane/EtOAc)

실험 절차

Preparation according to Preparation 1 using 5-bromo-2-hydroxybenzaldehyde (6 g, 29 mmol), (R)-glycidyltosylate (6.7 g, 29 mmol), K2CO3 (4.9 g, 35 mmol) and DMF (12 ml). The combined organic phases were washed with LiCl (5%, 100 ml), HCl (1 N, 100 ml), brine (100 ml) and were evaporated to dryness. The residue was purified by flash column chromatography (isooctane/EtOAc) to give the crude title compound (6.8 g). MS m/z (rel. intensity, 70 eV) 257 (M+, 38), 256 (M+, 39), 200 (bp), 199 (87), 57 (88).

출처

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