反応 #56391

反応方程式

Sodium

Ethyl 2,2-dichloro-acetate

4-Methoxyphenol

→

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

収率 76.7%

溶媒

diethyl ether

ethanol

ethanol

ethanol

ethanol

反応条件

後処理

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
   その他is driven off under reduced pressure (20 mmHg) at 40° C.
6. 6
   洗浄The organic phase is washed with 0.1 N sodium hydroxide solution (100 cc) and with water (2×100 cc)
7. 7
   乾燥is then dried over sodium sulphate
8. 8
   ろ過filtered
9. 9
   濃縮concentrated to dryness under reduced pressure (20 mmHg) at 40° C

実験手順

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.

出典