Реакция #56391

Уравнение реакции

Sodium

Ethyl 2,2-dichloro-acetate

4-Methoxyphenol

→

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

Выход 76.7%

Растворители

diethyl ether

ethanol

ethanol

ethanol

ethanol

Условия реакции

Обработка

1. 1
   workup.ADDITIONis added
2. 2
   workup.ADDITIONis then added
3. 3
   Температураthe mixture is heated
4. 4
   Температураunder reflux for 20 hours
5. 5
   Другоеis driven off under reduced pressure (20 mmHg) at 40° C.
6. 6
   ПромывкаThe organic phase is washed with 0.1 N sodium hydroxide solution (100 cc) and with water (2×100 cc)
7. 7
   Сушкаis then dried over sodium sulphate
8. 8
   Фильтрацияfiltered
9. 9
   Концентрированиеconcentrated to dryness under reduced pressure (20 mmHg) at 40° C

Методика

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.

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