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Hydrochloric Acid → HCID 15670192、化合物

HRID 1646290
ノート
印刷プレビュー

反応式

HRID 1646290 の反応式
[Na+].C([S:5][CH2:6][CH:7]([CH2:20][C:21]1[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=1)[C:8]([NH:10][C:11]1[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=1)[C:14]([O-:16])=[O:15])=[O:9])(=O)C.[OH-].[Na+].Cl>O>[SH:5][CH2:6][CH:7]([CH2:20][C:21]1[CH:22]=[CH:23][C:24]([F:27])=[CH:25][CH:26]=1)[C:8]([NH:10][C:11]1[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=1)[C:14]([OH:16])=[O:15])=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 23701009HCID 23701009、化合物

生成物 1

HCID 15670192HCID 15670192、化合物収率 59.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

3-[[2-Acetylthiomethyl-3-(4-fluorophenyl)propionyl]amino]benzoic acid sodium salt (compound- of Example 40) (1.2 g) is dissolved in water (20 ml), and the mixture is adjusted to pH 12.0 with 10% aqueous sodium hydroxide solution under nitrogen. After reacting at room temperature for one hour, the reaction mixture is adjusted to pH 2.5 with 10% hydrochloric acid. The mixture is extracted with ethyl acetate (50 ml). The extract is washed with water and ethyl acetate is distilled off. The residue is purified by a medium pressure column chromatography with CHP-20P (eluant, water-dioxane). The fractions containing the desired compound are collected and lyophilized to give the title compound (0.6 g).

後処理

  1. extractionThe mixture is extracted with ethyl acetate (50 ml)
  2. washThe extract is washed with water and ethyl acetate
  3. distillationis distilled off
  4. customThe residue is purified by a medium pressure column chromatography with CHP-20P (eluant, water-dioxane)
  5. additionThe fractions containing the desired compound
  6. customare collected

出典と根拠

ORDレコード
ord-735a818164874fc797b0818f4880b5ca
出典データセット
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05179125

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート