P-Cresol → Ethyl 2,2-bis(4-methylphenoxy)acetate

HRID 28114노트

반응식

HRID 28114 반응식
[Na].[CH:2]1[C:7]([OH:8])=[CH:6][CH:5]=[C:4]([CH3:9])[CH:3]=1.Cl[CH:11](Cl)[C:12]([O:14][CH2:15][CH3:16])=[O:13]>C(O)C.C(OCC)C>[CH3:9][C:4]1[CH:5]=[CH:6][C:7]([O:8][CH:11]([O:8][C:7]2[CH:2]=[CH:3][C:4]([CH3:9])=[CH:5][CH:6]=2)[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:2][CH:3]=1

참가 물질

6

반응물 3

HCID 2879P-CresolHCID 10808Ethyl dichloroacetateHCID 5360545Sodium

생성물 1

HCID 23338923Ethyl 2,2-bis(4-methylphenoxy)acetate수율 77.3%

시약·촉매·용매 2

HCID 702Ethanol용매3회HCID 3283Diethyl Ether용매

반응 조건

온도
20 °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.

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 20 hours
  3. temperatureto cool
  4. customThe white precipitate obtained
  5. filtrationis filtered off
  6. concentrationthe filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
  7. customThe oil thus obtained
  8. washwashed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time)
  9. dry with materialThe ethereal phase is then dried over anhydrous sodium sulphate
  10. filtrationfiltered
  11. concentrationconcentrated to dryness under reduced pressure (20 mmHg) at 40° C

출처 및 근거

ORD 기록
ord-b1d0998d3cf545b793e561524dc0c9a6
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04225589

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