反应详情

温度

133.5 °C

To a stirred solution of 3-(chloromethyl)pyridine hydrochloride (5.17 g, 31.5 mmol) in water (8 mL) was added K2CO3 (4.34 g, 31.5 mmol) portionwise. The resulting mixture was extracted three times with diethyl ether. The extracts were combined and washed twice with brine, dried and concentrated. The residue (3.25 g, 25.5 mmol) was dissolved in xylene (30 mL) and Ph3P (6.70 g, 25.5 mmol) was added. The mixture was heated at 133-134° C. overnight and then cooled to ambient temperature. The solid product was filtered, washed with toluene, and dried under vacuum to give (3-pyridylmethyl)triphenylphosphonium chloride (5.86 g, 48%) as a pinkish solid.

1. extractionThe resulting mixture was extracted three times with diethyl ether
2. washwashed twice with brine
3. customdried
4. concentrationconcentrated
5. temperaturecooled to ambient temperature
6. filtrationThe solid product was filtered
7. washwashed with toluene
8. customdried under vacuum