반응 #55460

ord-ea1e65734a0e40e6bc9129376137757b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThe reaction mixture is diluted with 50 ml
  2. 2
    세척of water and is washed with ether
  3. 3
    추출the oil which separates is extracted into chloroform
  4. 4
    세척The extract is washed with water
  5. 5
    건조dried over anhydrous sodium sulfate
  6. 6
    여과filtered
  7. 7
    농축concentrated in vacuo

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.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04220654uspto-grants-1980_09