HRID2227245

反应详情

EQUATION

反应方程式

HRID 2227245 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6-phenyl-3(2H)-pyridazinone potassium salt (10 mmol) (prepared from 6-phenyl-3(2H)-pyridazinone (1.72 g; 10 mmol) and KOH in methanol (0.56 g; 10 mmol), 2-bromoethanol (12 mmol), TBAB (1.19 g; 4 mmol) and atomised KOH (11 mmol) in toluene (60 mL) was stirred at room temperature for 6 hours. The reaction mixture was filtered, the filtrate was washed successively with 5% NaOH solution, 10% HCl solution and lastly water. The organic extracts were dried over anhydrous Na2SO4 and concentrated to dryness, and the obtained residue was purified by flash chromatography (CH22Cl2MeOH 98:2), yielding the title product (1.9 g).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. washthe filtrate was washed successively with 5% NaOH solution, 10% HCl solution and lastly water
  3. dry with materialThe organic extracts were dried over anhydrous Na2SO4
  4. concentrationconcentrated to dryness
  5. customthe obtained residue was purified by flash chromatography (CH22Cl2MeOH 98:2)