反应详情

温度

90 °C

A mixture of 1,2-dibromo-3,5-difluorobenzene (4.5 g), 3,3-dimethoxyprop-1-ene (5.1 mL), tetrabutylammonium chloride (4.6 g) and triethylamine (3.5 mL) in N,N-dimethylformamide (50 mL) is purged with nitrogen for 20 minutes. Palladium-(II)-acetate (111 mg) is added and the mixture heated for 16 hours at 90° C. After cooling the mixture is partitioned between aqueous HCl (1 M) and diethyl ether, the organic layer dried (Na2SO4), volatiles evaporated under reduced pressure and the residue purified by column chromatography (silica gel; hexane:ethyl acetate 98:2→80:20) to give the title compound (Yield 3.6 g).

1. customis purged with nitrogen for 20 minutes
2. additionPalladium-(II)-acetate (111 mg) is added
3. temperatureAfter cooling the mixture
4. customis partitioned between aqueous HCl (1 M) and diethyl ether
5. dry with materialthe organic layer dried (Na2SO4)
6. customvolatiles evaporated under reduced pressure
7. customthe residue purified by column chromatography (silica gel; hexane:ethyl acetate 98:2→80:20)