Реакция #2348083

ord-93ec32f1bdfe4060aa5a89d1c5a72512

Уравнение реакции

CCOP(c1ccccc1)c1ccccc1
Ethyl diphenylphosphinite
FC(F)(F)CI
1,1,1-trifluoro-2-iodoethane
O=P(CC(F)(F)F)(c1ccccc1)c1ccccc1
2,2,2-trifluoroethyl diphenylphosphine oxide
Выход 51.0%

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe resulting mixture was purified by means
  2. 2
    Другоеof fraction-collecting column chromatography
  3. 3
    Другоеfurther purified by recrystallization from a mixed solvent of toluene and heptane (volume ratio of toluene:heptane=1:1)
  4. 4
    Другоеdried

Методика

Ethyl diphenylphosphinite (b1; 20.0 g) and 1,1,1-trifluoro-2-iodoethane (b2; 36.5 g) were put into a reaction vessel under an argon atmosphere, and stirred at room temperature for 4 days. The resulting mixture was purified by means of fraction-collecting column chromatography using ethyl acetate as the eluent and silica gel as the stationary phase powder, and further purified by recrystallization from a mixed solvent of toluene and heptane (volume ratio of toluene:heptane=1:1), and then dried, whereby 12.6 g of 2,2,2-trifluoroethyl diphenylphosphine oxide (b3) was obtained. The yield based on the compound (b1) was 51.2%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07846514B2uspto-grants-2010_12