Reaktion #1074524

ord-796bebe025cd41308d8a054d48c52d4a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    TemperaturAfter cooling
  3. 3
    Filtrationthe solids were filtered off
  4. 4
    Waschenwashed with acetone
  5. 5
    SonstigeThe combined organic fractions were evaporated to dryness
  6. 6
    workup.ADDITIONDiethyl ether was added to the resultant oil
  7. 7
    Sonstigewas stored at 4° C
  8. 8
    SonstigeThe title compound precipitated
  9. 9
    Filtrationwas collected by filtration

Vorschrift

A mixture of 12-bromododecan-1-ol (15 g, 57 mmol, see Example 1 above), 4-hydroxy-benzaldehyde (6.9 g, 57 mmol), potassium carbonate (excess), potassium iodide (trace) and tetra-n-butylammonium iodide (trace) was heated at reflux in methyl ethyl ketone (50 ml) for 16 hours. After cooling, the solids were filtered off and washed with acetone. The combined organic fractions were evaporated to dryness. Diethyl ether was added to the resultant oil and the solution was stored at 4° C. The title compound precipitated and was collected by filtration.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06630128B1uspto-grants-2003_10