反応 #53321

ord-d5e7066c8825462298cfd234519deab5

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The precipitate was filtered off
  2. 2
    その他dried
  3. 3
    workup.DISSOLUTIONdissolved in DCM
  4. 4
    洗浄The organic solution was washed with NH3 (aq.) (excess)
  5. 5
    乾燥dried with potassium carbonate
  6. 6
    ろ過filtered
  7. 7
    その他the solvent was evaporated

実験手順

Iodomethane (1.76 ml) was added to 4-cyanophenyl-thiourea (5.0 g) in acetone (100 ml). The reaction mixture was stirred overnight at RT. The precipitate was filtered off, dried and dissolved in DCM. The organic solution was washed with NH3 (aq.) (excess), dried with potassium carbonate, filtered, and the solvent was evaporated, yielding 4.53 g (84%, white solid) of methyl N′-(4-cyanophenyl)-carbamimidothioate (intermediate 6).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06858609B2uspto-grants-2005_02