Reaktion #1182353

ord-49df06bc6d5846ab81d7002d5fec2e82

Lösungsmittel

Reaktionsbedingungen

Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to room temperature
  2. 2
    Sonstigepartitioned between water and ethyl acetate
  3. 3
    WaschenThe organic layer was washed with water for 3 times
  4. 4
    Trocknendried over anhydrous Na2SO4
  5. 5
    Einengenconcentrated
  6. 6
    SonstigeThe residue was purified by column chromatography

Vorschrift

To a mixture of 5-bromo-2-hydroxy-benzaldehyde (14 g, 70 mmol), KI (5 g) and K2CO3 (19 g, 140 mmol) in DMF (100 mL) was added toluene-4-sulfonic acid 3-ethyl-oxetan-3-ylmethyl ester (19 g, 70 mmol). The mixture was heated at 140° C. for 2 h, and then cooled to room temperature, partitioned between water and ethyl acetate. The organic layer was washed with water for 3 times, dried over anhydrous Na2SO4 and concentrated. The residue was purified by column chromatography to give the title compound (10 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08134001B2uspto-grants-2012_03