Reaktion #214312

ord-d09e1adc98e14711a1ffe0ba13241011

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    TemperaturAt the end of this period, the reaction mixture was cooled to room temperature
  2. 2
    ExtraktionThe resulting mixture was then extracted with methylene chloride
  3. 3
    SonstigeThe extract was dried
  4. 4
    Sonstigestripped of methylene chloride by use of a rotary evaporator
  5. 5
    workup.DISTILLATIONThe residue was distilled

Vorschrift

2-(1-Bromoethyl)-1,3-dioxolane (60 grams) and 40% aqueous methylamine (160 ml) were charged into a pressure vessel and heated, with agitation, for a period of about 16 hours at a temperature of about 100° C. under autogeneous pressure. At the end of this period, the reaction mixture was cooled to room temperature and 16 grams of NaOH added. The resulting mixture was then extracted with methylene chloride. The extract was dried, then stripped of methylene chloride by use of a rotary evaporator. The residue was distilled to yield the desired product N-[1-(1,3-dioxolan-2-yl)ethyl]methylamine as a fraction boiling at 60° C.-65° C. at about 12 mm Hg pressure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04255182uspto-grants-1981_03