반응 #40787

반응 방정식

Malononitril

1-iodo-3,3,3-trifluoropropane

NaH

→

oil

수율 16.4%

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

수율 16.4%

용매

THF

반응 조건

후처리

1. 1
   온도the mixture was cooled with an ice/salt bath
2. 2
   기타the temperature below 5° C
3. 3
   기타evaporated under reduced pressure
4. 4
   기타The crude material was purified by flash chromatography
5. 5
   세척eluting with DCM

실험 절차

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)

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