Reacción #434800

ord-794f4d0144e84dccaef656b3b1c84b40

Disolventes

Condiciones de reacción

Temperatura
20°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONwere charged to a 1 l stirrer
  2. 2
    Temperaturaheated
  3. 3
    Otro(110° C.)
  4. 4
    Temperaturaunder reflux for a period of 4 h
  5. 5
    Lavadowashed until neutral with sodium carbonate solution and water
  6. 6
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

Procedimiento

100 g (0.63 mol) of (±)-1-phenyl-1,2-ethanediol (3) (87% pure according to GC) according to Example 1, 200 ml of toluene, 32 g (0.24 mol) of paraldehyde and 1 g of para-toluenesulfonic acid were charged to a 1 l stirrer, heated to boiling (110° C.) and stirred under reflux for a period of 4 h. A total of 10 ml of water were eliminated. After this time, the mixture was cooled to 20° C. and washed until neutral with sodium carbonate solution and water, and the solvent was distilled off under reduced pressure, leaving 103 g of crude product (85.3% pure according to GC). GC conditions see Example 2.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07176176B2uspto-grants-2007_02