反応 #55460

ord-ea1e65734a0e40e6bc9129376137757b

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONThe reaction mixture is diluted with 50 ml
  2. 2
    洗浄of water and is washed with ether
  3. 3
    抽出the oil which separates is extracted into chloroform
  4. 4
    洗浄The extract is washed with water
  5. 5
    乾燥dried over anhydrous sodium sulfate
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated in vacuo

実験手順

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.).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04220654uspto-grants-1980_09