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

HRID 488690
ノート
印刷プレビュー

反応式

HRID 488690 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒

1
HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2391c019b6244bd3b15092931190dbb3
出典データセット
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE038921E1

反応ノート

読み込み中…

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