反应 #56391

反应方程式

Sodium

Ethyl 2,2-dichloro-acetate

4-Methoxyphenol

→

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

收率 76.7%

溶剂

diethyl ether

ethanol

ethanol

ethanol

ethanol

反应条件

后处理

1. 1
   workup.ADDITIONis added
2. 2
   workup.ADDITIONis then added
3. 3
   温度the mixture is heated
4. 4
   温度under reflux for 20 hours
5. 5
   其他is driven off under reduced pressure (20 mmHg) at 40° C.
6. 6
   洗涤The organic phase is washed with 0.1 N sodium hydroxide solution (100 cc) and with water (2×100 cc)
7. 7
   干燥is then dried over sodium sulphate
8. 8
   过滤filtered
9. 9
   浓缩concentrated to dryness under reduced pressure (20 mmHg) at 40° C

实验过程

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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