HRID1500919

反应详情

EQUATION

反应方程式

HRID 1500919 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 4-chloro-1-fluoro-2-nitrobenzene (9.2 g, 52.4 mmol), 4-amino-1-(4-methoxybenzyl)pyrrolidin-2-one (11.5 g, 52.4 mmol) and K2CO3 (14.5 g, 105 mmol) in 300 mL of anhydrous CH3CN was heated with stirring at 50° C. for 16 hours. The reaction mixture was filtered and the filter cake was dissolved with H2O (400 mL), and extracted with EtOAc (200 mL×4). The organic layers and the filtrate was combined and concentrated in vacuo to 50 mL. The precipitate was collected by filtration and washed with 10 mL of PE to afford 4-[(4-chloro-2-nitrophenyl)amino]-1-(4-methoxybenzyl)pyrrolidin-2-one as an orange solid (15.8 g, yield: 80.2%).

WORKUP

后处理

  1. temperaturewas heated
  2. filtrationThe reaction mixture was filtered
  3. dissolutionthe filter cake was dissolved with H2O (400 mL)
  4. extractionextracted with EtOAc (200 mL×4)
  5. concentrationconcentrated in vacuo to 50 mL
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with 10 mL of PE