Reaktion #56323

ord-e99f9d76b08a481ba3c31cb20e20a62f

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 (5.0 grams) was added to the filtrate
  5. 5
    workup.DISTILLATIONvacuum distilled
  6. 6
    Sonstigethe fraction boiling at 120° C. and 0.07 mm of Hg pressure was collected

Vorschrift

2-Methoxyaniline (99 grams; 0.6 moles) and sodium carbonate (31.6 grams) were charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. 2-Bromomethyl-4-methyl-1,3-dioxolane (25 ml) was added and the reaction mixture was heated at a temperature of about 100° C. for a period of about 4 hours. After this time the reaction mixture was filtered and additional sodium carbonate (5.0 grams) was added to the filtrate. The mixture was then vacuum distilled and the fraction boiling at 120° C. and 0.07 mm of Hg pressure was collected to yield the desired product N-(4-methyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline.

Quelle

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