반응 #82263

ord-3d0d18ea8fa64a2b90025bea52f01bed

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the solution was refluxed
  2. 2
    온도under heating for 3 hours
  3. 3
    온도After cooling
  4. 4
    workup.DISTILLATIONdistilling off the solvent
  5. 5
    workup.DISSOLUTIONthe resulting residue was dissolved in ethyl acetate
  6. 6
    세척washed with water
  7. 7
    기타dried
  8. 8
    workup.DISTILLATIONAfter distilling off the solvent
  9. 9
    기타the crystals thus precipitated
  10. 10
    여과were collected by filtration

실험 절차

3.42 g of 3,4-diaminobenzonitrile and 4.06 g of ethyl chloroacetoimidate hydrochloride were dissolved in 100 ml of ethanol, and the solution was refluxed under heating for 3 hours. After cooling and distilling off the solvent, the resulting residue was dissolved in ethyl acetate, washed with water, and then dried. After distilling off the solvent, the crystals thus precipitated were collected by filtration to obtain 2.7 g of 2-chloromethyl-5-benzimidazolecarbonitrile.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05620991uspto-grants-1997_04