Reaktion #1102759
ord-3e02bb80784a42de9000b85da69e6e35
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperatursubsequently refluxed for 0.5 hrs
- 2TemperaturAfter cooling to room temperature
- 3SonstigeThe solid material that precipitated
- 4Sonstigewas collected by suction
- 5Sonstigerecrystallized from a minimum of boiling methanol
Vorschrift
A mixture of 2-benzyloxy-5-bromobenzaldehyde (0.10 mol), malonic acid (15.0 g), and piperidine (2.0 ml) in 150 ml of pyridine was first heated at 90° C. for 90 min and subsequently refluxed for 0.5 hrs. After cooling to room temperature, the reaction was poured on a mixture of ice (1 kg) and concentrated aqueous hydrochloric acid (250 ml). The solid material that precipitated after stirring for 2 hrs. was collected by suction and recrystallized from a minimum of boiling methanol.