反应 #56393

反应方程式

Sodium

ethyl dichloroacetate

4-methylthiophenol

→

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

收率 68.0%

溶剂

diethyl ether

methanol

methanol

methanol

反应条件

后处理

1. 1
   温度to cool
2. 2
   其他the white precipitate obtained
3. 3
   过滤is filtered off
4. 4
   浓缩the filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
5. 5
   其他The oil obtained
6. 6
   洗涤washed four times with N sodium hydroxide solution (50 cc each time) and four times with distilled water (50 cc each time)
7. 7
   干燥The ethereal phase is dried over anhydrous sodium sulphate
8. 8
   过滤filtered
9. 9
   workup.ADDITIONtreated with animal charcoal
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 (3.54 g) is dissolved in methanol (140 cc) and a solution of 4-methylthiophenol (21.8 g) in methanol (25 cc) is added. The mixture is stirred for 1 hour at 20° C. and a solution of ethyl dichloroacetate (12.5 g) in methanol (30 cc) is then added. The mixture is 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 obtained is taken up in diethyl ether (250 cc) and washed four times with N sodium hydroxide solution (50 cc each time) and four times with distilled water (50 cc each time). The ethereal phase is dried over anhydrous sodium sulphate, filtered, treated with animal charcoal, filtered and concentrated to dryness under reduced pressure (20 mmHg) at 40° C. Ethyl 2,2-bis(4-methylthiophenoxy)acetate (18 g) is thus obtained as a yellow oil.

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