反应 #55460

ord-ea1e65734a0e40e6bc9129376137757b

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.).

来源

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