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Potassium Iodide → Ethyl 4-[6-acetyl-3-[2-(4-acetyl-3-hydroxy-2-propylphenylthio)-ethoxy]-2-propylphenoxy]butyrate

HRID 488690
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HRID 488690 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]([O:22][CH2:23][CH2:24]Cl)=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[OH:26][C:27]1[C:32]([CH2:33][CH2:34][CH3:35])=[C:31]([SH:36])[CH:30]=[CH:29][C:28]=1[C:37](=[O:39])[CH3:38].[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[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]([O:22][CH2:23][CH2:24][S:36][C:31]2[CH:30]=[CH:29][C:28]([C:37](=[O:39])[CH3:38])=[C:27]([OH:26])[C:32]=2[CH2:33][CH2:34][CH3:35])=[CH:6][CH:5]=1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 132955181-(2-Hydroxy-3-propyl-4-sulfanylphenyl)ethan-1-oneHCID 15712390Ethyl 4-[6-acetyl-3-(2-chloroethoxy)-2-propylphenoxy]butyrate

생성물 1

HCID 15712393Ethyl 4-[6-acetyl-3-[2-(4-acetyl-3-hydroxy-2-propylphenylthio)-ethoxy]-2-propylphenoxy]butyrate수율 82.8%

시약·촉매·용매

1
HCID 180Acetone용매

실험 절차

A mixture of ethyl 4-[6-acetyl-3-(2-chloroethoxy)-2-propylphenoxy]butyrate (0.60 g), (2-hydroxy-4-mercapto-3-propylphenyl)ethanone (0.51 g), potassium iodide (0.1 g) and potassium carbonate (0.65 g) in acetone (40 ml) was heated and refluxed with stirring for 19 hours. After cooled, inorganic materials were separated by filtration and the filtrate was concentrated. The resultant residue was separated and purified through silica gel column chromatography (eluting with benzene:ethyl acetate=15:1, then 9:1) to give the title compound (0.73 g, 82.8%) as brown oil.

후처리

  1. temperaturewas heated
  2. temperaturerefluxed
  3. temperatureAfter cooled
  4. custominorganic materials were separated by filtration
  5. concentrationthe filtrate was concentrated
  6. customThe resultant residue was separated
  7. custompurified through silica gel column chromatography (
  8. washeluting with benzene

출처 및 근거

ORD 기록
ord-2391c019b6244bd3b15092931190dbb3
출처 데이터셋
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE038921E1

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