Reacción #55310

ord-ccbdcc529e104ca9a8cdaf4b5e1e4621

Ecuación de reacción

C1COCCO1
1,4-dioxane
N#Cc1nc[nH]c1C#N
4,5-dicyanoimidazole
CCN(CC)CC
triethylamine
CN(C)C(=O)Cl
dimethylcarbamoyl chloride
CN(C)C(=O)n1cnc(C#N)c1C#N
1-(N,N-Dimethylcarbamoyl)-4,5-dicyanoimidazole

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturarefluxed for 3 days
  2. 2
    Otroevaporated to dryness
  3. 3
    workup.STIRRINGThe residue is stirred in 50 ml of ethyl acetate
  4. 4
    OtroThe organic layer is separated
  5. 5
    Lavadowashed
  6. 6
    Otrodried
  7. 7
    Otroevaporated
  8. 8
    Otroto give 8 g

Procedimiento

To 50 ml of dry 1,4-dioxane 6.0 g (0.05 mole) of 4,5-dicyanoimidazole, 5.0 g (0.05 mole) of triethylamine and 6.0 g (0.055 mole) of dimethylcarbamoyl chloride are added in succession at room temperature. This mixture is stirred and refluxed for 3 days, cooled to room temperature and evaporated to dryness. The residue is stirred in 50 ml of ethyl acetate and 50 ml water. The organic layer is separated, washed, dried and evaporated to give 8 g. (85%) of white product.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04220466uspto-grants-1980_09