반응 #55310

ord-ccbdcc529e104ca9a8cdaf4b5e1e4621

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 3 days
  2. 2
    기타evaporated to dryness
  3. 3
    workup.STIRRINGThe residue is stirred in 50 ml of ethyl acetate
  4. 4
    기타The organic layer is separated
  5. 5
    세척washed
  6. 6
    기타dried
  7. 7
    기타evaporated
  8. 8
    기타to give 8 g

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04220466uspto-grants-1980_09