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

HRID 27183
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HRID 27183 반응식
[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
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참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water
용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-31bea89f94fe486db9b7de125628220f
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04220654

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