HRID347735

反应详情

EQUATION

反应方程式

HRID 347735 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,4-Dichloropyrimidine (500 mg, 3.36 mmol), 2,5-dimethylaniline (407 mg, 3.36 mmol) and triethylamine (0.51 ml, 3.69 mmol) were dissolved in EtOH (5 ml) with stirring. The reaction mixture was heated at reflux for 12 hours, cooled and evaporated onto silica (5 ml). The residue was purified by column chromatography and eluted with EtOAc (30%): isohexane to give the title product as a waxy solid on evaporation (514 mg, 66%). NMR (300 MHz): 2.1 (s, 3H), 2.27 (s, 3H), 6.42 (d. 1H), 6.99 (d, 1H), 7.08 (s, 1H). 7.18 (d, 1H), 8.03 (d, 1H), 9.45 (s, 1H); m/z: (ES+) 234.3 (MH+).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 12 hours
  3. temperaturecooled
  4. customevaporated onto silica (5 ml)
  5. customThe residue was purified by column chromatography
  6. washeluted with EtOAc (30%)