تفاعل #56391

معادلة التفاعل

Sodium

Ethyl 2,2-dichloro-acetate

4-Methoxyphenol

→

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

المردود 76.7%

المذيبات

diethyl ether

ethanol

ethanol

ethanol

ethanol

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONis added
2. 2
   workup.ADDITIONis then added
3. 3
   درجة الحرارةthe mixture is heated
4. 4
   درجة الحرارةunder reflux for 20 hours
5. 5
   أخرىis driven off under reduced pressure (20 mmHg) at 40° C.
6. 6
   غسيلThe organic phase is washed with 0.1 N sodium hydroxide solution (100 cc) and with water (2×100 cc)
7. 7
   تجفيفis then dried over sodium sulphate
8. 8
   ترشيحfiltered
9. 9
   تركيزconcentrated to dryness under reduced pressure (20 mmHg) at 40° C

الإجراء التجريبي

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.

المصدر