Reacción #214312

ord-d09e1adc98e14711a1ffe0ba13241011

Condiciones de reacción

Temperatura
100°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

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

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04255182uspto-grants-1981_03