HRID263437

反应详情

EQUATION

反应方程式

HRID 263437 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

2-Nitro-4-(4-fluorophenoxy)toluene (11.8 g, 47.7 mmol), was dissolved in dimethylformamide (90.0 mL) under N2 atmosphere. Dimethylformamide dimethyl acetal (20.2 mL, 143 mmol), and pyrrolidine (4.0 mL, 47.4 mmol) were added via syringe and the reaction mixture was heated at 110° C. for 3 hours. The reaction mixture was cooled to ambient temperature and partitioned between H2O and ether. The organic phase was washed with H2O. The combined aqueous extracts were washed with ether. The ether extracts were combined and dried over Na2SO4, filtered, and concentrated in vacuo to give a viscous oil (16.1 g) which was used without further purification.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to ambient temperature
  2. custompartitioned between H2O and ether
  3. washThe organic phase was washed with H2O
  4. washThe combined aqueous extracts were washed with ether
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo