反应详情

A 250 mL round bottom flask was charged with 2-chloro-6-methylpyrazine (4.0 g, 0.031 mol), 1-methylpiperazine (12.4 g, 0.125 mol) and EtOH (100 mL). The resulting mixture was heated at reflux overnight. Work-up: the solvent was evaporated. The residue was mixed with saturated aqueous NaHCO3 (100 mL) and then extracted with CH2Cl2 (100 mL×3). The combined organic layers were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was further purified by flash column chromatography on silica gel with 4% MeOH in CH2Cl2, to afford 2.7 g (45%) of the product as a white solid. MS m/z: 193 (M+H+).

1. temperatureThe resulting mixture was heated
2. temperatureat reflux overnight
3. customthe solvent was evaporated
4. additionThe residue was mixed with saturated aqueous NaHCO3 (100 mL)
5. extractionextracted with CH2Cl2 (100 mL×3)
6. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
7. concentrationconcentrated in vacuo
8. customThe residue was further purified by flash column chromatography on silica gel with 4% MeOH in CH2Cl2