反应详情

A mixture of Pd2 dba3 (1.924 g, 2.101 mmol), and PPh3 (2.204 g, 8.404 mmol) was dissolved in toluene (200 mL), degassed and then stirred 10 minutes at ambient temperature. A solution of 1-bromo-2,4-difluoro-5-nitrobenzene (10 g, 42.02 mmol) in toluene (200 mL) was then added to the above solution, followed by tributyl(vinyl)stannane (18.40 mL, 63.03 mmol). The mixture was refluxed for 2 hours, then poured into a mixture of aqueous NaF and diethyl ether. The residue was purified using silica gel column chromatography with 5-10-20% acetone in hexanes to provide 1,5-difluoro-2-nitro-4-vinylbenzene (6 g, 32.41 mmol, 77.13% yield) as yellow oil.

1. customdegassed
2. temperatureThe mixture was refluxed for 2 hours
3. customThe residue was purified