Reaktion #1182353
ord-49df06bc6d5846ab81d7002d5fec2e82
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturcooled to room temperature
- 2Sonstigepartitioned between water and ethyl acetate
- 3WaschenThe organic layer was washed with water for 3 times
- 4Trocknendried over anhydrous Na2SO4
- 5Einengenconcentrated
- 6SonstigeThe 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).