반응 #56391

반응 방정식

Sodium

Ethyl 2,2-dichloro-acetate

4-Methoxyphenol

→

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

수율 76.7%

용매

diethyl ether

ethanol

ethanol

ethanol

ethanol

반응 조건

후처리

1. 1
   workup.ADDITIONis added
2. 2
   workup.ADDITIONis then added
3. 3
   온도the mixture is heated
4. 4
   온도under reflux for 20 hours
5. 5
   기타is driven off under reduced pressure (20 mmHg) at 40° C.
6. 6
   세척The organic phase is washed with 0.1 N sodium hydroxide solution (100 cc) and with water (2×100 cc)
7. 7
   건조is then dried over sodium sulphate
8. 8
   여과filtered
9. 9
   농축concentrated to dryness under reduced pressure (20 mmHg) at 40° C

실험 절차

Sodium (5.4 g) is dissolved in absolute ethanol (160 cc). 4-Methoxyphenol (29.2 g) dissolved in absolute ethanol (20 cc) is added. The mixture is stirred for 1 hour at ambient temperature. Ethyl 2,2-dichloro-acetate (20 g) dissolved in absolute ethanol (20 cc) is then added and the mixture is heated under reflux for 20 hours. The ethanol is driven off under reduced pressure (20 mmHg) at 40° C. and the residue is taken up in diethyl ether (100 cc). The organic phase is washed with 0.1 N sodium hydroxide solution (100 cc) and with water (2×100 cc) and is then dried over sodium sulphate, filtered and concentrated to dryness under reduced pressure (20 mmHg) at 40° C. Ethyl 2,2-bis(4-methoxyphenoxy)-acetate (30 g) is thus obtained in the form of an oil.

출처