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Sodium Hydroxide → 4-[4-Acetyl-3-[2-[2-(4-acetyl-3-hydroxy-2-propylphenoxy)ethoxy]ethoxy]-2-propylphenoxy]butanoic acid

HRID 2231471
ノート
印刷プレビュー

反応式

HRID 2231471 の反応式
C([O:3][C:4](=[O:41])[CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=[O:17])[CH3:16])=[C:11]([O:18][CH2:19][CH2:20][O:21][CH2:22][CH2:23][O:24][C:25]2[CH:30]=[CH:29][C:28]([C:31](=[O:33])[CH3:32])=[C:27]([OH:34])[C:26]=2[CH2:35][CH2:36][CH3:37])[C:10]=1[CH2:38][CH2:39][CH3:40])C.[OH-].[Na+]>CO>[C:15]([C:12]1[CH:13]=[CH:14][C:9]([O:8][CH2:7][CH2:6][CH2:5][C:4]([OH:41])=[O:3])=[C:10]([CH2:38][CH2:39][CH3:40])[C:11]=1[O:18][CH2:19][CH2:20][O:21][CH2:22][CH2:23][O:24][C:25]1[CH:30]=[CH:29][C:28]([C:31](=[O:33])[CH3:32])=[C:27]([OH:34])[C:26]=1[CH2:35][CH2:36][CH3:37])(=[O:17])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 143299774-[4-Acetyl-3-[2-[2-(4-acetyl-3-hydroxy-2-propylphenoxy)ethoxy]ethoxy]-2-propylphenoxy]butanoic acid ethyl ester

生成物 1

HCID 133891614-[4-Acetyl-3-[2-[2-(4-acetyl-3-hydroxy-2-propylphenoxy)ethoxy]ethoxy]-2-propylphenoxy]butanoic acid収率 81.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 0.526 g (0.0009 mol) of 4-[4-acetyl-3-[2-[2-(4-acetyl-3-hydroxy-2-propylphenoxy)ethoxy]ethoxy]-2-propylphenoxy]butanoic acid ethyl ester in 23 ml of methanol was added 23 ml (0.023 mol) of 1N sodium hydroxide. The mixture was stirred at 25° for 6 hours and the methanol was removed in vacuo. The aqueous solution was acidified to pH 3, the precipitate was dissolved in ethyl acetate and washed with sodium chloride solution. The oil obtained on concentration of the ethyl acetate was purified by column chromatography, eluting with 50% ethyl acetate-hexane and ethyl acetate to yield 0.4 g (80% yield) of 4-[4-acetyl-3-[2-[2-(4-acetyl-3-hydroxy-2-propylphenoxy)ethoxy]ethoxy]-2-propylphenoxy]butanoic acid as a pale yellow oil which solidified (melting point 52°-58°).

後処理

  1. customthe methanol was removed in vacuo
  2. dissolutionthe precipitate was dissolved in ethyl acetate
  3. washwashed with sodium chloride solution
  4. customThe oil obtained on concentration of the ethyl acetate
  5. customwas purified by column chromatography
  6. washeluting with 50% ethyl acetate-hexane and ethyl acetate

出典と根拠

ORDレコード
ord-87ecbd1d2a88492c934145d9a37cc637
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

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