تفاعل #56393

معادلة التفاعل

Sodium

ethyl dichloroacetate

4-methylthiophenol

→

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

المردود 68.0%

المذيبات

diethyl ether

methanol

methanol

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto cool
2. 2
   أخرىthe white precipitate obtained
3. 3
   ترشيحis filtered off
4. 4
   تركيزthe filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
5. 5
   أخرىThe oil obtained
6. 6
   غسيلwashed four times with N sodium hydroxide solution (50 cc each time) and four times with distilled water (50 cc each time)
7. 7
   تجفيفThe ethereal phase is dried over anhydrous sodium sulphate
8. 8
   ترشيحfiltered
9. 9
   workup.ADDITIONtreated with animal charcoal
10. 10
    ترشيحfiltered
11. 11
    تركيزconcentrated to dryness under reduced pressure (20 mmHg) at 40° C

الإجراء التجريبي

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.

المصدر