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

HRID 28115

반응식

HRID 28115 반응식
[Na].[CH3:2][C:3]1[CH:8]=[CH:7][C:6]([SH:9])=[CH:5][CH:4]=1.Cl[CH:11](Cl)[C:12]([O:14][CH2:15][CH3:16])=[O:13]>CO.C(OCC)C>[CH3:2][C:3]1[CH:8]=[CH:7][C:6]([S:9][CH:11]([S:9][C:6]2[CH:7]=[CH:8][C:3]([CH3:2])=[CH:4][CH:5]=2)[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:5][CH:4]=1

참가 물질

6

반응물 3

HCID 78114-MethylbenzenethiolHCID 10808Ethyl dichloroacetateHCID 5360545Sodium

생성물 1

HCID 13107767Ethyl 2,2-bis(4-methylthiophenoxy)acetate수율 68%

시약·촉매·용매 2

HCID 887Methanol용매3회HCID 3283Diethyl Ether용매

반응 조건

온도
20 °C

실험 절차

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.

후처리

  1. temperatureto cool
  2. customthe white precipitate obtained
  3. filtrationis filtered off
  4. concentrationthe filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
  5. customThe oil obtained
  6. washwashed four times with N sodium hydroxide solution (50 cc each time) and four times with distilled water (50 cc each time)
  7. dry with materialThe ethereal phase is dried over anhydrous sodium sulphate
  8. filtrationfiltered
  9. additiontreated with animal charcoal
  10. filtrationfiltered
  11. concentrationconcentrated to dryness under reduced pressure (20 mmHg) at 40° C

출처 및 근거

ORD 기록
ord-6bb31a9cb3cd4b5eaac488e1d6f003df
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04225589

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