HRID1799190

反应详情

EQUATION

反应方程式

HRID 1799190 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of (4R)-4-(2-bromo-4-chlorophenyl)pyrrolidin-2-one (140 mg, 0.51 mmol), Pd(OAc)2 (34 mg, 0.15 mmol) and triphenylphosphine (0.3 mmol) in DMF (1 mL) was added styrene (0.17 mL, 2 mmol) followed by diisopropylethylamine (0.17 mL, 1.02 mmol) under a N2 atmosphere. The reaction mixture was heated to 90° C. overnight. The mixture was then cooled to room temperature and diluted with 1N HCl aq. solution (10 mL) and extracted with ethyl acetate (3×30 mL). The combined organic phases were washed with brine (3×30 mL) and dried over MgSO4. The solvent was removed in vacuo to provide 4-[2-((1E)-2-phenylvinyl)-4-chlorophenyl](4R)pyrrolidin-2-one (3a) (120 mg). MS (ESI) m/z 284.02 (M+H)+.

WORKUP

后处理

  1. temperatureThe mixture was then cooled to room temperature
  2. extractionextracted with ethyl acetate (3×30 mL)
  3. washThe combined organic phases were washed with brine (3×30 mL)
  4. dry with materialdried over MgSO4
  5. customThe solvent was removed in vacuo