HRID1398220

反应详情

EQUATION

反应方程式

HRID 1398220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a mixture of 1-(4-bromo-2-fluorophenyl)-3-methyl-1H-1,2,4-triazole (5.5 g), tris(dibenzylideneacetone)dipalladium(0) (393 mg), 1,1′-bis(diphenylphosphino)ferrocene (476 mg) and zinc powder (169 mg) in N,N-dimethylacetamide (20 mL) was added zinc(II) cyanide (1.5 g) at room temperature, and the mixture was stirred at 120° C. for 1 hr. To the reaction mixture were added ethyl acetate, water and aqueous ammonia. The organic layer was separated, washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (3.84 g).

WORKUP

后处理

  1. customThe organic layer was separated
  2. washwashed with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)