Reacción #6290
ord-71e3ae6057b24905aebe514e2d6cc7ed
Ecuación de reacción
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Temperatura
5°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1Temperaturacooled
- 2workup.DISSOLUTIONAfter the salts had dissolved
- 3FiltraciónThe solid product was filtered
- 4Lavadowashed twice with water
- 5Otrorecrystallized (still wet) from 250 ml of ethanol
- 6TemperaturaCooling 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.