HRID1824061

反应详情

EQUATION

反应方程式

HRID 1824061 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

POBr3 (573 mg) was added to the solution of 3-(2,4-dichlorophenyl)-2,5-dimethylpyrazine 1-oxide (270 mg) and proton sponge (197 mg) in CH2Cl2 at 0° C. The reaction mixture was warmed to r.t. for 10 h. The reaction mixture was washed with 1N HCl, NaHCO3 and brine, dried (MgSO4), filtered and concentrated. Flash chromatography (silica gel Heptane:EtOAC 100:1) gave the title compound (110 mg, 35%) and 3-(2,4-dichlorophenyl)-2,5-dimethylpyrazine (100 mg, 38%). 1H NMR (CDCl3) δ 2.40, 2.71, 7.28, 7.40, 7.54; MS (ESI+) for C12H9Cl2N2Br1 m/z 333.0 (M+H)+.

WORKUP

后处理

  1. washThe reaction mixture was washed with 1N HCl, NaHCO3 and brine
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated