HRID2235389

反应详情

EQUATION

反应方程式

HRID 2235389 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-fluoro-2-methyl-pyridine (0.75 g) (J. Med. Chem. 1989, 32, 1970) in CCl4 (25 ml) is added N-bromosuccinimide (0.96 g; 5.4 mmol) and benzoyl peroxide (200 mg; 0.8 mmol). The mixture is heated at reflux for 3 h, cooled to RT and stirred for additional 12 h. The suspension is filtered through celite and the filtrate is washed with Na2SO4, dried over MgSO4 and evaporated. The crude material (0.22 g) containing approximately 50% of the dibrominated species is used without further purification.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureat reflux for 3 h
  3. filtrationThe suspension is filtered through celite
  4. washthe filtrate is washed with Na2SO4
  5. dry with materialdried over MgSO4
  6. customevaporated
  7. additionThe crude material (0.22 g) containing approximately 50% of the dibrominated species
  8. customis used without further purification