反应详情

To a stirred suspension of sodium hydride (0.54 g, 12.3 mmol) in THF (40 ml) at 20° C. was added 2-methylimidazole in portions over 45 min. 3-Bromo-5-(chloromethyl)-pyridine (1 g, 4.1 mmol) in ethanol (8 ml) was then added and this mixture was heated under reflux for 1 h under an argon atmosphere. After cooling and evaporation of solvents the residue was suspended in MeOH, filtered and adsorbed onto silica gel. Chromatographic elution with CH2Cl2/(2M NH3 MeOH)=98:2 afforded the title compound (0.56 g, 53%) as a yellow oil. MS: m/e=251.0 (M+).

1. temperaturethis mixture was heated
2. temperatureunder reflux for 1 h under an argon atmosphere
3. temperatureAfter cooling
4. customevaporation of solvents the residue
5. filtrationfiltered
6. washChromatographic elution with CH2Cl2/(2M NH3 MeOH)=98:2