反応 #56179

ord-dffacfefda164193be659bca22101673

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture was refluxed until clear solution
  2. 2
    その他was obtained
  3. 3
    温度The mixture was cooled
  4. 4
    その他the solid which crystallised
  5. 5
    その他was removed by filtration
  6. 6
    その他The mother liquors, after evaporation and crystallisation of the residual oil
  7. 7
    その他yielded 5.5 g

実験手順

3,5-Dichloro-2-amino pyridine (8.15, 0.05 mol) was treated with thiophosgenes (10% soln. in toluene, 55 ml). The mixture was refluxed until clear solution was obtained and no further hydrochloric acid gas was being evolved. The mixture was cooled, and the solid which crystallised was removed by filtration. The mother liquors, after evaporation and crystallisation of the residual oil, yielded 5.5 g. (55%) of the required isothiocyanate as pale yellow needles m. pt. 45°-6°.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04224331uspto-grants-1980_09