反応 #40787

反応方程式

Malononitril

1-iodo-3,3,3-trifluoropropane

NaH

→

oil

収率 16.4%

2,2-Bis-(2,2,2-trifluoro-ethyl)-malononitrile

収率 16.4%

溶媒

THF

反応条件

後処理

1. 1
   温度the mixture was cooled with an ice/salt bath
2. 2
   その他the temperature below 5° C
3. 3
   その他evaporated under reduced pressure
4. 4
   その他The crude material was purified by flash chromatography
5. 5
   洗浄eluting with DCM

実験手順

Malononitril (20.15 mmol) and 1-iodo-3,3,3-trifluoropropane (42.65 mmol) were dissolved in 30 ml dry THF, and the mixture was cooled with an ice/salt bath. 1.61 g NaH (40.3 mmol) was added portionwise, keeping the temperature below 5° C. The reaction mixture was stirred at room temperature for 2 hours and evaporated under reduced pressure. The crude material was purified by flash chromatography eluting with DCM, yielding 0.76 grams of an oil. 1H NMR (400 MHz, CDCl3) δ 2.62-2.49 (m, 4H), 2.31-2.24 (m, 4H)

出典