反応 #56392

反応方程式

Sodium

ethyl dichloroacetate

para-cresol

→

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

収率 77.3%

溶媒

diethyl ether

ethanol

ethanol

ethanol

反応条件

後処理

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
   その他The white precipitate obtained
5. 5
   ろ過is filtered off
6. 6
   濃縮the filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
7. 7
   その他The oil thus obtained
8. 8
   洗浄washed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time)
9. 9
   乾燥The ethereal phase is then dried over anhydrous sodium sulphate
10. 10
    ろ過filtered
11. 11
    濃縮concentrated to dryness under reduced pressure (20 mmHg) at 40° C

実験手順

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.

出典