Reacción #55460

ord-ea1e65734a0e40e6bc9129376137757b

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONThe reaction mixture is diluted with 50 ml
  2. 2
    Lavadoof water and is washed with ether
  3. 3
    Extracciónthe oil which separates is extracted into chloroform
  4. 4
    LavadoThe extract is washed with water
  5. 5
    Secadodried over anhydrous sodium sulfate
  6. 6
    Filtraciónfiltered
  7. 7
    Concentraciónconcentrated in vacuo

Procedimiento

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.).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04220654uspto-grants-1980_09