HRID991624

反应详情

EQUATION

反应方程式

HRID 991624 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-phenoxyethylamine (2.65 g, 19.3 mmol), 2,3-dichloropyrazine (2.88 g, 19.3 mmol) and K2CO3 (2.67 g, 19.3 mmol) in acetonitrile (8 mL) was stirred in a sealed tube for 12 h at room temperature, and for a further 9.5 h at 80° C. The reaction mixture was diluted with ether, filtered, and concentrated. The residue was purified by chromatography on silica gel using n-hexane/EtOAc (7:3) as eluent to give 2.36 g (49%) of the title compound as a yellowish oil that solidified on standing: mp 51-53° C.; HRMS m/z calcd for C12H12ClN30 (M)+ 249.0669, found 249.0659. Anal. (Cl2H12ClN30) C, H, N.

WORKUP

后处理

  1. waitfor a further 9.5 h at 80° C
  2. filtrationfiltered
  3. concentrationconcentrated
  4. customThe residue was purified by chromatography on silica gel