Reaktion #1573608

ord-0b045545a2a040428890c9c9319df889

Reaktionsbedingungen

Temperatur
75°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeInto a 2 L round-bottom flask was placed
  2. 2
    TemperaturThe flask was heated
  3. 3
    Einengenthe contents were concentrated on a Rotavap at 75° C.
  4. 4
    workup.ADDITIONTo the residue, methyl tert-butyl ether (800 mL) was added
  5. 5
    workup.STIRRINGThe slurry was vigorously stirred by a mechanical stirrer for 12 h
  6. 6
    Filtrationfiltered
  7. 7
    Waschenwashed with 3 portions (400 mL each) of methyl tert-butyl ether
  8. 8
    Sonstigedried in vacuum

Vorschrift

Into a 2 L round-bottom flask was placed hexadecyl bromide (250 g), 2-methoxypropanol (250 mL), and triethylamine (200 mL). The flask was heated without stirring at 75° C. for 96 h and the contents were concentrated on a Rotavap at 75° C. and 20 mbar. To the residue, methyl tert-butyl ether (800 mL) was added. The slurry was vigorously stirred by a mechanical stirrer for 12 h, filtered, washed with 3 portions (400 mL each) of methyl tert-butyl ether, and dried in vacuum to obtain the product as a white solid in nearly quantitative yield.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09427406B2uspto-grants-2016_08