Thioglycolic Acid → 4-(4-Methylphenylsulfonyl)phenylthio acetic acid

HRID 2392

반응식

HRID 2392 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C:11]2[CH:16]=[CH:15][C:14](Cl)=[CH:13][CH:12]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.C(O)(=O)C[SH:20].[OH-].[K+].[CH3:25][CH:26]([OH:28])C>CN(C)C=O.O>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C:11]2[CH:16]=[CH:15][C:14]([CH2:25][C:26]([OH:28])=[S:20])=[CH:13][CH:12]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 1133Thioglycolic AcidHCID 3776IsopropanolHCID 14797Potassium HydroxideHCID 2862191-Chloro-4-(4-methylbenzene-1-sulfonyl)benzene

생성물 1

HCID 1784183824-(4-Methylphenylsulfonyl)phenylthio acetic acid

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

In 250 ml of N,N-dimethylformamide, 140 g of 4-methyl-4'-chlorodiphenylsulfone was dissolved, and further 77 g of thioglycolic acid and 71 g of 85% potassium hydroxide pellet were added and stirred for 6 hours at 120° C. The reaction mixture was poured into 2-propanol and filtered off to obtain a precipitate. After the precipitate obtained was dissolved in water and then the insoluble matter was filtered off, 150 ml of concentrated chloric acid and 500 g of ice were added therein. The formed white crystal was filtered off and washed with water and further recrystallized with a mixed solvent of n-hexane and ethylacetate to obtain 110 g of the intended 4-(4-methylphenylsulfonyl)phenylthio acetic acid.

후처리

  1. filtrationfiltered off
  2. customto obtain a precipitate
  3. customAfter the precipitate obtained
  4. filtrationthe insoluble matter was filtered off
  5. addition150 ml of concentrated chloric acid and 500 g of ice were added
  6. filtrationThe formed white crystal was filtered off
  7. washwashed with water
  8. customfurther recrystallized with a mixed solvent of n-hexane and ethylacetate

출처 및 근거

ORD 기록
ord-ceb80269f1a342758c971e5e753be1b3
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728879

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