Reaktion #56392

Reaktionsgleichung

Sodium

ethyl dichloroacetate

para-cresol

→

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

Ausbeute 77.3%

Lösungsmittel

diethyl ether

ethanol

ethanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is heated
2. 2
   Temperaturunder reflux for 20 hours
3. 3
   Temperaturto cool
4. 4
   SonstigeThe white precipitate obtained
5. 5
   Filtrationis filtered off
6. 6
   Einengenthe filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
7. 7
   SonstigeThe oil thus obtained
8. 8
   Waschenwashed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time)
9. 9
   TrocknenThe ethereal phase is then dried over anhydrous sodium sulphate
10. 10
    Filtrationfiltered
11. 11
    Einengenconcentrated to dryness under reduced pressure (20 mmHg) at 40° C

Vorschrift

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.

Quelle