Reaktion #50707

ord-c98a8881a4794c408626888262f8759e

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool
  2. 2
    Extraktionthe mixture extracted with diethyl ether (2×40 ml)
  3. 3
    SonstigeThe extracts were dried
  4. 4
    Filtrationfiltered
  5. 5
    Sonstigeevaporated to a yellow solid
  6. 6
    SonstigeRecrystallisation from methanol (25 ml)

Vorschrift

8-Phenyloctyl bromide (2.69 g, 10 mmol) was added to a stirred mixture of 5-methyl-2-hydroxy-1,3-benzenedicarboxaldehyde (1.64 g, 10 mmol) and anhydrous potassium carbonate (1.38 g, 10 mmol) in dry dimethylformamide (20 ml) at room temperature under nitrogen. The suspension was heated to 80° C. for 3 hours then allowed to cool. Water (40 ml) was added and the mixture extracted with diethyl ether (2×40 ml). The extracts were dried, filtered and evaporated to a yellow solid. Recrystallisation from methanol (25 ml) gave the title product as pale yellow crystals, m.p. 59° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05428065uspto-grants-1995_06