HRID919293

反应详情

EQUATION

反应方程式

HRID 919293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution 6-chloropyridazin-3(2H)-one (130 mg, 1.0 mmol) in acetonitrile (3.0 mL) was added K2CO3 (437 mg, 3.16 mmol), CH3I (299 mg, 2.11 mmol), the reaction mixture was stirred at reflux for 2 h. The mixture was cooled to ambient temperature, diluted with EtOAc (20 mL), washed with sodium bicarbonate (10 mL) and brine (10 mL), dried over MgSO4, filtered and concentrated. The residue was purified with silica gel column (Petroleum ether:ethyl acetate=4:1) to obtained product: LC/MS m/z=145 (M+H)+.

WORKUP

后处理

  1. temperatureat reflux for 2 h
  2. washwashed with sodium bicarbonate (10 mL) and brine (10 mL)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified with silica gel column (Petroleum ether:ethyl acetate=4:1)
  7. customto obtained product