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Ethylene Glycol → HCID 54524012、化合物

HRID 257498
ノート
印刷プレビュー

反応式

HRID 257498 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[N:10]([CH2:11][C:12]([OH:14])=[O:13])[N:9]=[N:8][N:7]=1.S(=O)(=O)(O)O.[CH2:20](O)[CH2:21][OH:22]>>[OH:22][CH2:21][CH2:20][O:13][C:12](=[O:14])[CH2:11][N:10]1[C:6]([C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)=[N:7][N:8]=[N:9]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 174Ethylene GlycolHCID 1118Sulfuric AcidHCID 2159421H-Tetrazole-1-acetic acid, 5-(2-thienyl)-

生成物 1

HCID 54524012HCID 54524012、化合物収率 88.5%

反応条件

温度
90 °C

実験手順

To a solution of a 1 g (4.7 mM) of [5-(2-thienyl)tetrazol-1-yl] acetic acid in 5 ml of ethylene glycol was added 0.5 ml of sulfuric acid. After the addition, the mixture was stirred at 90° C. for 2.5 hrs. The mixture was then poured into ice-water and extracted with ethyl acetate. The organic phase was washed with water, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The resultant residue was subjected to silica gel column chromatography (eluent: chloroform/methyl alcohol=50/1) for separation and purification, to give 1 g (yield 88.5%) of [5-(2-thienyl)tetrazol-1-yl] acetic acid 2-hydroxyethyl ester.

後処理

  1. additionAfter the addition
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resultant residue was subjected to silica gel column chromatography (eluent: chloroform/methyl alcohol=50/1) for separation and purification

出典と根拠

ORDレコード
ord-e1dc088cfc2649cb98c60310af1e22ba
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05262433

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート