反应详情

Add sodium hydride (54 mg, 2.25 mmol) to 2.5 mL ethylene glycol at 0° C. and stir for 30 min at RT. Add 5-bromomethyl-2-fluoro-4-iodo-pyridine (0.69 g, 2.14 mmol) and heat it to 120° C. for 30 min. Cool to RT, dilute with 70 mL of water, and extract with ether (3×50 mL). Combine organic layers, wash with saturated aqueous sodium chloride, thy over MgSO4, and remove the solvent. Purify by chromatography with diethylether to obtain the title compound (240 mg, 38%). MS (ES) m/z 296 [M+1]+.

1. temperatureCool to RT
2. extractionextract with ether (3×50 mL)
3. washCombine organic layers, wash with saturated aqueous sodium chloride, thy over MgSO4
4. customremove the solvent
5. customPurify by chromatography with diethylether