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

HRID 27182

반응식

HRID 27182 반응식
C([C:3]1([C:9]2[N:10]=[CH:11][N:12]([CH2:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[C:13]=2[CH3:14])[CH2:7][C:6](=[O:8])[CH2:5][S:4]1)C.O>>[CH2:15]([N:12]1[C:13]([CH3:14])=[C:9]([CH:3]2[CH2:7][C:6](=[O:8])[CH2:5][S:4]2)[N:10]=[CH:11]1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

참가 물질

3

반응물 2

HCID 962WaterHCID 86737180Ethyl 2-(1-benzyl-5-methyl-4-imidazolyl)-4-oxotetrahydrothiophene

생성물 1

HCID 233436792-(1-Benzyl-5-methyl-4-imidazolyl)-4-oxotetrahydrothiophene

실험 절차

Ethyl 2-(1-benzyl-5-methyl-4-imidazolyl)-4-oxotetrahydrothiophene-5(and/or 3)-carboxylate (12.6 g., 0.037 mole) is dissolved in 20 ml. of water containing concentrated sulfuric acid (1.11 ml., 0.02 mole) and the solution is refluxed for 31/4 hours. The reaction mixture is diluted with 50 ml. of water and is washed with ether. The aqueous layer is made basic with sodium carbonate and the oil which separates is extracted into chloroform. The extract is washed with water, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The product 2-(1-benzyl-5-methyl-4-imidazolyl)-4-oxotetrahydrothiophene is isolated a brown gum (7.8 g.).

후처리

  1. additionThe reaction mixture is diluted with 50 ml
  2. washof water and is washed with ether
  3. extractionthe oil which separates is extracted into chloroform
  4. washThe extract is washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ea1e65734a0e40e6bc9129376137757b
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04220654

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