反応 #2348083

反応方程式

Ethyl diphenylphosphinite

1,1,1-trifluoro-2-iodoethane

→

2,2,2-trifluoroethyl diphenylphosphine oxide

収率 51.0%

反応条件

後処理

1. 1
   その他The resulting mixture was purified by means
2. 2
   その他of fraction-collecting column chromatography
3. 3
   その他further purified by recrystallization from a mixed solvent of toluene and heptane (volume ratio of toluene:heptane=1:1)
4. 4
   その他dried

実験手順

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%.

出典