反応 #63082

ord-291331072b234f3eae842ce3a0c3e233

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他evaporated to dryness
  2. 2
    その他The residue was partitioned between water and ethyl acetate
  3. 3
    乾燥the ethyl acetate phase was dried
  4. 4
    その他evaporated to dryness
  5. 5
    その他The residue was recrystallised from a mixture of acetone and light petroleum ether (b.p. 60°-80°)

実験手順

2,2,2-Trifluoroethylisothiocyanate (2.12 g.) was added to a mixture of 2,2,2-trifluoroethylamine hydrochloride (1.36 g), triethylamine (1.01 g) and acetonitrile (10 ml.), and the mixture stirred at room temperature for 4 hours and then evaporated to dryness. The residue was partitioned between water and ethyl acetate, and the ethyl acetate phase was dried and evaporated to dryness. The residue was recrystallised from a mixture of acetone and light petroleum ether (b.p. 60°-80°) to give 1,3-di(2,2,2-trifluoroethyl)thiourea, m.p. 152°-153°.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04762932uspto-grants-1988_08