Reaktion #56312

ord-b450100da9fe427db4334b43432f4259

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeequipped with a mechanical stirrer
  2. 2
    Temperaturthermometer and reflux condenser
  3. 3
    FiltrationAfter this time the reaction mixture was filtered
  4. 4
    workup.ADDITIONadditional sodium carbonate (5.00 grams) was added to the filtrate
  5. 5
    workup.DISTILLATIONThe mixture was then distilled under reduced pressure

Vorschrift

2-Methoxyaniline (87 ml; 0.7 mole) and sodium carbonate (31.66 grams) were charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. 2-Bromomethyl-4,5-dimethyl-1,3-dioxolane (25 mls) was added and the reaction mixture was heated at a temperature of 100° C. for a period of about 4 hours. After this time the reaction mixture was filtered and additional sodium carbonate (5.00 grams) was added to the filtrate. The mixture was then distilled under reduced pressure to yield the desired product N-(4,5-dimethyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline boiling at 125° to 128° C. at 0.1 mm of Hg pressure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04225335uspto-grants-1980_09