Reaktion #43900

ord-4587e73c346047e7ae98bdbb2f4f0c05

Reaktionsbedingungen

Temperatur
95°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA 2 L four-necked flask equipped with a stirrer
  2. 2
    SonstigeAfter the elapse of 45 min, it
  3. 3
    Temperaturthe mixture was cooled
  4. 4
    Sonstigeseparated into two layers
  5. 5
    workup.DISTILLATIONThe thus separated organic layer was subjected to distillation treatment

Vorschrift

A 2 L four-necked flask equipped with a stirrer, a thermometer and a reflux condenser was charged with 762 g (6.0 mol) of n-octanal, 520 g (6.4 mol) of a 37% by mass formaldehyde aqueous solution, 15 g (0.33 mol) of dibutyl amine and 10 g (0.06 mol) of decanoic acid, and the contents in the flask were stirred while heating at 95° C. After the elapse of 45 min, it was confirmed that no n-octanal was present in the raw mixture, and then the mixture was cooled and separated into two layers. The thus separated organic layer was subjected to distillation treatment, thereby obtaining 790 g (5.4 mol) of a-methylene octanal (purity as measured by gas chromatography: 95%) (yield based on theoretical amount: 90%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732644B2uspto-grants-2010_06