反应详情

A mixture of 2-bromomethyl-2,3-dihydrobenzo[1,4]dioxine (500 mg, 2.18 mmol) and 3-phenyl-pyridine (339 mg, 2.18 mmol) in xylene (2 ml) was refluxed for 4 h. After cooling, the solvent was decanted to give the crude oily pyridinium salt, which was dissolved in MeOH (5 ml). NaBH4 (330 mg, 4 eq) was added in small portions to the cooled mixture. After stirring for 2 h at RT, MeOH was evaporated, water was added and the mixture extracted with EtOAc. Drying (Na2SO4) and evaporation gave the crude product, which was purified by flash chromatography (heptane/EtOAc).

1. temperaturewas refluxed for 4 h
2. temperatureAfter cooling
3. customthe solvent was decanted
4. customto give the crude oily pyridinium salt, which
5. customMeOH was evaporated
6. additionwater was added
7. extractionthe mixture extracted with EtOAc
8. customDrying
9. custom(Na2SO4) and evaporation