Reacción #56392

Ecuación de reacción

Sodium

ethyl dichloroacetate

para-cresol

→

Ethyl 2,2-bis(4-methylphenoxy)acetate

Rendimiento 77.3%

Disolventes

diethyl ether

ethanol

ethanol

ethanol

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe mixture is heated
2. 2
   Temperaturaunder reflux for 20 hours
3. 3
   Temperaturato cool
4. 4
   OtroThe white precipitate obtained
5. 5
   Filtraciónis filtered off
6. 6
   Concentraciónthe filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
7. 7
   OtroThe oil thus obtained
8. 8
   Lavadowashed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time)
9. 9
   SecadoThe ethereal phase is then dried over anhydrous sodium sulphate
10. 10
    Filtraciónfiltered
11. 11
    Concentraciónconcentrated to dryness under reduced pressure (20 mmHg) at 40° C

Procedimiento

Sodium (5.7 g) is dissolved in ethanol (160 cc), and a solution of para-cresol (27 g) in ethanol (20 cc) is added. The mixture is stirred for 1 hour at 20° C. and ethyl dichloroacetate (20 g) in solution in ethanol (20 cc) is then added. The mixture is heated under reflux for 20 hours and then allowed to cool. The white precipitate obtained is filtered off and the filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C. The oil thus obtained is taken up in diethyl ether (300 cc) and washed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time). The ethereal phase is then dried over anhydrous sodium sulphate, filtered, and concentrated to dryness under reduced pressure (20 mmHg) at 40° C. Ethyl 2,2-bis(4-methylphenoxy)acetate (29 g) is thus obtained as a yellow oil.

Fuente