HRID624656

反应详情

EQUATION

反应方程式

HRID 624656 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl formate (330 mg, 4.46 mmol) and succinonitrile (300 mg, 3.75 mmol) in toluene (1561 μl) was added dropwise to a suspension of sodium methanolate (215 mg, 3.97 mmol) in toluene (1561 μl) at 0° C. After being stirred at RT for 3 h, the reaction mixture was treated with 1,1,1-trifluoro-2-methylpropan-2-amine (486 mg, 3.82 mmol) and acetic acid (255 μl, 4.46 mmol) then heated at 120° C. for 3 h. After being cooled to RT, the reaction mixture was washed with brine, then dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to afford the title compound as a brown oil, which was used without further purification.

WORKUP

后处理

  1. temperaturethen heated at 120° C. for 3 h
  2. temperatureAfter being cooled to RT
  3. washthe reaction mixture was washed with brine
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure