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Potassium Carbonate → HCID 14329995、化合物

HRID 2231468
ノート
印刷プレビュー

反応式

HRID 2231468 の反応式
[Cl:1][C:2]1[C:3]([OH:15])=[C:4]([CH2:12][CH2:13][CH3:14])[C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1.[CH2:16]([O:18][C:19](=[O:45])[CH2:20][O:21][C:22]1[CH:27]=[CH:26][C:25]([C:28](=[O:30])[CH3:29])=[C:24]([O:31][CH2:32][CH2:33][O:34][CH2:35][CH2:36]OS(C)(=O)=O)[C:23]=1[CH2:42][CH2:43][CH3:44])[CH3:17].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.CN(C)C=O>[CH2:16]([O:18][C:19](=[O:45])[CH2:20][O:21][C:22]1[CH:27]=[CH:26][C:25]([C:28](=[O:30])[CH3:29])=[C:24]([O:31][CH2:32][CH2:33][O:34][CH2:35][CH2:36][O:15][C:3]2[C:2]([Cl:1])=[CH:7][C:6]([C:8](=[O:10])[CH3:9])=[C:5]([OH:11])[C:4]=2[CH2:12][CH2:13][CH3:14])[C:23]=1[CH2:42][CH2:43][CH3:44])[CH3:17]
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 3

HCID 11430Potassium CarbonateHCID 133891721-(5-Chloro-2,4-dihydroxy-3-propylphenyl)ethanoneHCID 54223276HCID 54223276、化合物

生成物 1

HCID 14329995HCID 14329995、化合物収率 31%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 6228
Dimethylformamide
溶媒

実験手順

A mixture of 0.512 g (0.00224 mol) of 1-(5-chloro-2,4-dihydroxy-3-propylphenyl)ethanone, 1.000 g (0.00224 mol) of [4-acetyl-3-[2-[2-[(methylsulfonyl)oxy]ethoxy]ethoxy]-2-propylphenoxy]acetic acid ethyl ester and 0.620 g (0.00448 mol) of anhydrous potassium carbonate in 20 ml of anhydrous acetone and 10 ml of anhydrous dimethylformamide was stirred at reflux for 24 hours. The reaction mixture was filtered and concentrated in vacuo to an oil which was treated with ethyl acetate and sodium chloride solution. The crude oil obtained on concentration of the ethyl acetate was purified by column chromatography, eluting with 20-30% ethyl acetate-hexane to yield 0.400 g (31% yield) of [4-acetyl-3-[2-[2-(4-acetyl-6-chloro-3-hydroxy-2-propylphenoxy)ethoxy]ethoxy]2-propylphenoxy]acetic acid ethyl ester as a pale yellow oil.

後処理

  1. temperatureat reflux for 24 hours
  2. filtrationThe reaction mixture was filtered
  3. concentrationconcentrated in vacuo to an oil which
  4. additionwas treated with ethyl acetate and sodium chloride solution
  5. customThe crude oil obtained on concentration of the ethyl acetate
  6. customwas purified by column chromatography
  7. washeluting with 20-30% ethyl acetate-hexane

出典と根拠

ORDレコード
ord-2b3a6ea34220440a9e13f6ba7a207c9d
出典データセット
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04782176

反応ノート

読み込み中…

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