Reaktion #2395429

ord-6a293618d42c438798e20d405389667a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture was heated
  2. 2
    Temperaturat reflux under Dean-Stark conditions for 8 h
  3. 3
    WaschenAt this time, the cooled solution was washed with 2.5 N aqueous NaOH (200 mL), water (4×200 mL) and brine (200 mL)
  4. 4
    Trocknendried (K2CO3)
  5. 5
    Einengenconcentrated in vacuo

Vorschrift

3-Bromo-5-iodo-4-methylthiophene-2-carbaldehyde (27 g, 82 mmol), ethylene glycol (5.9 mL, 110 mmol) and p-toluenesulfonic acid monohydrate (0.50 g, 2.6 mmol) were combined in benzene (200 mL) and the mixture was heated at reflux under Dean-Stark conditions for 8 h. At this time, the cooled solution was washed with 2.5 N aqueous NaOH (200 mL), water (4×200 mL) and brine (200 mL), dried (K2CO3) and concentrated in vacuo to give the title compound (29 g, 94%) as an orange oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06835745B2uspto-grants-2004_12