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Sulfuric Acid → HCID 15712395, 화합물

HRID 704119
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HRID 704119 반응식
[C:1]([C:4]1[C:9]([O:10][CH2:11][CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:8]([CH2:19][CH2:20][CH3:21])[C:7]([S:22]C(=O)N(C)C)=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[OH-].[K+].S(=O)(=O)(O)O>C(O)C>[C:1]([C:4]1[C:9]([O:10][CH2:11][CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:8]([CH2:19][CH2:20][CH3:21])[C:7]([SH:22])=[CH:6][CH:5]=1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 14797Potassium HydroxideHCID 15712394Ethyl 4-(6-acetyl-3-(N,N-dimethylcarbamoylthio)-2-propylphenoxy)butyrate

생성물 1

HCID 15712395HCID 15712395, 화합물수율 89.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethyl 4-(6-acetyl-3-(N,N-dimethylcarbamoylthio)-2-propylphenoxy)butyrate (10.6 g) and potassium hydroxide (4.5 g) in ethanol (100 ml) were heated with stirring under refluxing for 1.5 hours. Ice water and conc. sulfuric acid were added thereto (pH 1), and then the mixture was subjected to extraction. The organic layer was washed with water and aqueous solution of sodium chloride, followed by being dried over sodium sulfate and then concentrated under a reduced pressure. To the resultant residue was added a mixture of ethanol (30 ml) and conc. sulfuric acid (0.5 ml), and the mixture was heated with stirring and refluxing for 1.5 hours. Ice water was added thereto and the mixture was extracted with ethyl acetate. The organic layer was washed with water and thereafter was dried over sodium sulfate, followed by being concentrated under a reduced pressure. Ethyl 4-(6-acetyl-3-mercapto-2-propylphenoxy)butyrate (7.8 g, 89.7%) was obtained as brown oil.

후처리

  1. temperatureunder refluxing for 1.5 hours
  2. extraction(pH 1), and then the mixture was subjected to extraction
  3. washThe organic layer was washed with water and aqueous solution of sodium chloride
  4. dry with materialby being dried over sodium sulfate
  5. concentrationconcentrated under a reduced pressure
  6. additionTo the resultant residue was added
  7. additiona mixture of ethanol (30 ml) and conc. sulfuric acid (0.5 ml)
  8. temperaturethe mixture was heated
  9. stirringwith stirring
  10. temperaturerefluxing for 1.5 hours
  11. additionIce water was added
  12. extractionthe mixture was extracted with ethyl acetate
  13. washThe organic layer was washed with water
  14. dry with materialwas dried over sodium sulfate
  15. concentrationby being concentrated under a reduced pressure

출처 및 근거

ORD 기록
ord-018da310761341ddb6be67fde1f51668
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04985585

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