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Ethanol → 2-(1-Benzyl-5-methyl-4-imidazolyl)-4-oxotetrahydrothiophene oxime

HRID 27183
ノート
印刷プレビュー

反応式

HRID 27183 の反応式
[CH2:1]([N:8]1[C:12]([CH3:13])=[C:11]([CH:14]2[CH2:18][C:17](=O)[CH2:16][S:15]2)[N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)C.Cl.[OH:24][NH2:25].C([O-])(=O)C.[Na+]>O>[CH2:1]([N:8]1[C:12]([CH3:13])=[C:11]([CH:14]2[CH2:18][C:17](=[N:25][OH:24])[CH2:16][S:15]2)[N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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 4

HCID 702EthanolHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 233436792-(1-Benzyl-5-methyl-4-imidazolyl)-4-oxotetrahydrothiophene

生成物 1

HCID 867371812-(1-Benzyl-5-methyl-4-imidazolyl)-4-oxotetrahydrothiophene oxime

試薬・触媒・溶媒 1

HCID 962Water
溶媒

実験手順

2-(1-Benzyl-5-methyl-4-imidazolyl)-4-oxotetrahydrothiophene (0.14 g., 0.5 mole) is dissolved in 1 ml. of ethanol and 1 ml. of water is added. Then hydroxyamine hydrochloride (38 mg., 0.55 mole) and sodium acetate (45 mg., 0.55 mole) are added. The mixture is stirred at room temperature overnight. The reaction mixture is concentrated in vacuo. The residue is triturated with chloroform and the mixture is filtered. The chloroform extract is dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The crude oxime, 2-(1-benzyl-5-methyl-4-imidazolyl)-4-oxotetrahydrothiophene oxime, is a brown viscous oil (0.15 g.).

後処理

  1. concentrationThe reaction mixture is concentrated in vacuo
  2. customThe residue is triturated with chloroform
  3. filtrationthe mixture is filtered
  4. extractionThe chloroform extract
  5. dry with materialis dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-31bea89f94fe486db9b7de125628220f
出典データセット
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04220654

反応ノート

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