HRID333365

反应详情

EQUATION

反应方程式

HRID 333365 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 6-fluorooxindole (3 g, 20 mmol) in THF (50 mL) at 0° C., was added 40 mL of 1M LHMDS in THF. The reaction mixture was stirred at 0° C. for 15 minutes. A solution of 4-bromo-5,5-dimethyl-5H-furan-2-one (5) (1.91 g, 10 mmol) in 5 mL of THF was added to the above reaction mixture. The reaction was stirred at 0° C. for further 30 minutes and then at room temperature for 2.5 hrs. To the reaction, 80 mL of 2M HCl was added. The resulting mixture was stirred at 50-55° C. for one hour, cooled down to room temperature, poured to 1000 mL of water and was stirred at room temperature for one hour. The precipitates formed were collected and washed with water, dried in vacuum to give the title compound as a yellow solid product (2.4 g, yield: 74%).

WORKUP

后处理

  1. stirringThe reaction was stirred at 0° C. for further 30 minutes
  2. waitat room temperature for 2.5 hrs
  3. additionwas added
  4. stirringThe resulting mixture was stirred at 50-55° C. for one hour
  5. temperaturecooled down to room temperature
  6. stirringwas stirred at room temperature for one hour
  7. customThe precipitates formed
  8. customwere collected
  9. washwashed with water
  10. customdried in vacuum