反应 #56392

反应方程式

Sodium

ethyl dichloroacetate

para-cresol

→

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

收率 77.3%

溶剂

diethyl ether

ethanol

ethanol

ethanol

反应条件

后处理

1. 1
   温度The mixture is heated
2. 2
   温度under reflux for 20 hours
3. 3
   温度to cool
4. 4
   其他The white precipitate obtained
5. 5
   过滤is filtered off
6. 6
   浓缩the filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
7. 7
   其他The oil thus obtained
8. 8
   洗涤washed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time)
9. 9
   干燥The ethereal phase is then dried over anhydrous sodium sulphate
10. 10
    过滤filtered
11. 11
    浓缩concentrated to dryness under reduced pressure (20 mmHg) at 40° C

实验过程

Sodium (5.7 g) is dissolved in ethanol (160 cc), and a solution of para-cresol (27 g) in ethanol (20 cc) is added. The mixture is stirred for 1 hour at 20° C. and ethyl dichloroacetate (20 g) in solution in ethanol (20 cc) is then added. The mixture is heated under reflux for 20 hours and then allowed to cool. The white precipitate obtained is filtered off and the filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C. The oil thus obtained is taken up in diethyl ether (300 cc) and washed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time). The ethereal phase is then dried over anhydrous sodium sulphate, filtered, and concentrated to dryness under reduced pressure (20 mmHg) at 40° C. Ethyl 2,2-bis(4-methylphenoxy)acetate (29 g) is thus obtained as a yellow oil.

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