Reaktion #67265

ord-03d4c742822045a0b1b79b9068c24fe4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigePreparation
  2. 2
    Extraktionthe solution was extracted with EtOAc (3×100 ml)
  3. 3
    WaschenThe combined organic phases were washed with LiCl (5%, 100 ml), HCl (1 N, 100 ml), brine
  4. 4
    Sonstigewere dried
  5. 5
    Einengenconcentrated

Vorschrift

Preparation according to Preparation 1 using 5-bromo-2-hydroxybenzaldehyde (6 g, 30 mmol), (S)-glycidyltosylate (8.2 g, 36 mmol), K2CO3 (4.9 g, 36 mmol) and DMF (12 ml). Water (100 ml) was added and the solution was extracted with EtOAc (3×100 ml). The combined organic phases were washed with LiCl (5%, 100 ml), HCl (1 N, 100 ml), brine, were dried and concentrated to give the crude title compound (8.3 g). MS m/z (rel. intensity, 70 eV) 257 (M+, 38), 256 (M+, 39), 200 (bp), 199 (87), 57 (88).

Quelle

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