HRID347735
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was heated
- temperatureat reflux for 12 hours
- temperaturecooled
- customevaporated onto silica (5 ml)
- customThe residue was purified by column chromatography
- washeluted with EtOAc (30%)