تفاعل #56392

ord-b1d0998d3cf545b793e561524dc0c9a6

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture is heated
  2. 2
    درجة الحرارةunder reflux for 20 hours
  3. 3
    درجة الحرارةto cool
  4. 4
    أخرىThe white precipitate obtained
  5. 5
    ترشيحis filtered off
  6. 6
    تركيزthe filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
  7. 7
    أخرىThe oil thus obtained
  8. 8
    غسيلwashed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time)
  9. 9
    تجفيفThe ethereal phase is then dried over anhydrous sodium sulphate
  10. 10
    ترشيحfiltered
  11. 11
    تركيزconcentrated to dryness under reduced pressure (20 mmHg) at 40° C

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04225589uspto-grants-1980_09