반응 #56392

반응 방정식

Sodium

ethyl dichloroacetate

para-cresol

→

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

수율 77.3%

용매

diethyl ether

ethanol

ethanol

ethanol

반응 조건

후처리

1. 1
   온도The mixture is heated
2. 2
   온도under reflux for 20 hours
3. 3
   온도to cool
4. 4
   기타The white precipitate obtained
5. 5
   여과is filtered off
6. 6
   농축the filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
7. 7
   기타The oil thus obtained
8. 8
   세척washed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time)
9. 9
   건조The ethereal phase is then dried over anhydrous sodium sulphate
10. 10
    여과filtered
11. 11
    농축concentrated to dryness under reduced pressure (20 mmHg) at 40° C

실험 절차

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.

출처