Methanol → 4-[5-(1-Imidazolylmethyl)-thien-2-yl]-4-oxobutyric acid

HRID 2164395ノート

反応式

HRID 2164395 の反応式
C[O:2][C:3](=[O:19])[CH2:4][CH2:5][C:6]([C:8]1[S:9][C:10]([CH2:13][C:14]2[NH:15][CH:16]=[CH:17][N:18]=2)=[CH:11][CH:12]=1)=[O:7].[OH-].[Na+].CO>O>[NH:18]1[CH:17]=[CH:16][N:15]=[C:14]1[CH2:13][C:10]1[S:9][C:8]([C:6](=[O:7])[CH2:5][CH2:4][C:3]([OH:19])=[O:2])=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 704876864-[5-(1-Imidazolylmethyl)-thien-2-yl]-4-oxo-butyric acid methyl ester

生成物 1

HCID 704292984-[5-(1-Imidazolylmethyl)-thien-2-yl]-4-oxobutyric acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 4.17 g of 4-[5-(1-imidazolylmethyl)-thien-2-yl]-4-oxo-butyric acid methyl ester, 0.8 g of sodium hydroxide and 20 ml of methanol is stirred at room temperature for 8 hours. The solvent is then stripped off and the residue is taken up in water. The solution is extracted several times with chloroform, and the chloroform phase is discarded. The aqueous solution is brought to about pH 7 with dilute hydrochloric acid and is concentrated to dryness. The residue is purified by column chromatography (silica gel/CHCl3 /methanol).

後処理

  1. extractionThe solution is extracted several times with chloroform
  2. concentrationis concentrated to dryness
  3. customThe residue is purified by column chromatography (silica gel/CHCl3 /methanol)

出典と根拠

ORDレコード
ord-ec16d96664ce4c5a8672c2a1e115f8be
出典データセット
uspto-grants-1985_03
特許番号
US04504479

反応ノート

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