HRID12509

反应详情

EQUATION

反应方程式

HRID 12509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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)

WORKUP

后处理

  1. temperaturethe mixture was cooled with an ice/salt bath
  2. customthe temperature below 5° C
  3. customevaporated under reduced pressure
  4. customThe crude material was purified by flash chromatography
  5. washeluting with DCM