HRID418570

反应详情

EQUATION

反应方程式

HRID 418570 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

A mixture of 7-chloro-2-(1-methyl-1H-imidazol-2-yl)thieno[3,2-b]pyridine (7) (1.0 g, 4 mmol), 2-fluoro-4-nitrophenol (0.942 g, 6 mmol) and K2CO3 (1.1 g, 8 mmol) in Ph2O (20 mL) was stirred at 200° C. for 24 h. The cooled reaction mixture was diluted with DCM (200 mL) and extracted with 1M HCl (200 mL). The aqueous phase was filtered through paper filter, basified (pH˜10) with conc. NH4OH to produce a cloudy mixture that was extracted with DCM. The organic phase was dried over anhydrous Na2SO4 and concentrated under pressure to give title compound 8 as an orange solid (0.667 g, 45% yield). MS (m/z): 371.0 (M+H).

WORKUP

后处理

  1. customThe cooled reaction mixture
  2. extractionextracted with 1M HCl (200 mL)
  3. filtrationThe aqueous phase was filtered through paper
  4. filtrationfilter
  5. customto produce a cloudy mixture that
  6. extractionwas extracted with DCM
  7. dry with materialThe organic phase was dried over anhydrous Na2SO4
  8. concentrationconcentrated under pressure