Reacción #57398

ord-929d3e8a42634e4ba14bfbfc337f01a7

Condiciones de reacción

Temperatura
190°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe mixture was cooled to 100° C.
  2. 2
    TemperaturaThe mixture was further cooled to 30° C.
  3. 3
    workup.STIRRINGThe mixture was stirred at the same temperature for 1 hr
  4. 4
    Filtraciónthe precipitated crystals were collected by filtration
  5. 5
    Lavadowashed with heptane

Procedimiento

A mixture of N-[2,3,6-trimethyl-4-[[2-methyl-3-(4-methylphenyl)-2-propenyl]oxy]phenyl]formamide (920 g), potassium carbonate (4.6 g) and N,N-dimethylaniline (2760 ml) was stirred at 190° C. for 4 hr under nitrogen stream. The mixture was cooled to 100° C. and heptane (1840 ml) was added dropwise thereto. The mixture was further cooled to 30° C. and heptane (3680 ml) was added dropwise thereto. The mixture was stirred at the same temperature for 1 hr, and the precipitated crystals were collected by filtration and washed with heptane to give the title compound (799.5 g, yield 86.9%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07420070B2uspto-grants-2008_09