Reacción #6290

ord-71e3ae6057b24905aebe514e2d6cc7ed

Disolventes

Condiciones de reacción

Temperatura
5°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturacooled
  2. 2
    workup.DISSOLUTIONAfter the salts had dissolved
  3. 3
    FiltraciónThe solid product was filtered
  4. 4
    Lavadowashed twice with water
  5. 5
    Otrorecrystallized (still wet) from 250 ml of ethanol
  6. 6
    TemperaturaCooling to 25° C.

Procedimiento

A slurry of 13.42 g of vanillin, 11.99 g of 1,10-dibromodecane, 6.16 g of anhydrous potassium carbonate and 300 ml of acetone was refluxed with stirring for 48 h, cooled and diluted with 400 ml of water. After the salts had dissolved, the mixture was chilled overnight at 5° C. The solid product was filtered, washed twice with water and recrystallized (still wet) from 250 ml of ethanol. Cooling to 25° C. gave 4.75 g of compound mp 93°-102° C., wetting at 65° C. (Further cooling of the mother liquors to 5° C. furnished 3.5 g of very impure materials, mp 55°-65° C.). Another recrystallization from 130 ml of ethanol raised the mp to 103°-105° C., slight wetting at 99° C.; 3.16 g.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05247055uspto-grants-1993_09