Реакция #63082

ord-291331072b234f3eae842ce3a0c3e233

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеevaporated to dryness
  2. 2
    ДругоеThe residue was partitioned between water and ethyl acetate
  3. 3
    Сушкаthe ethyl acetate phase was dried
  4. 4
    Другоеevaporated to dryness
  5. 5
    ДругоеThe residue was recrystallised from a mixture of acetone and light petroleum ether (b.p. 60°-80°)

Методика

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°.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04762932uspto-grants-1988_08