反应详情

A mixture of 2 g (8.03 mmol) of 4-(4-bromophenyl)phenol, 1.1 g (12.8 mmol) of methyl acrylate, 18 mg (0.08 mmol) of Palladium acetate, and 94 mg (0.31 mmol) of tri-(o-tolyl)phosphine in 3.7 ml of triethylamine was refluxed for 6 hours. A further 6 mg of Palladium acetate and 30 mg of tri-(o-tolyl)phosphine were added and heated for an hour, then a further 30 mg of Palladium acetate and 94 mg di tri-(o-toluyl)phosphine were added and heated for 3.5 hours. Then the reaction was acidified with 6M HCl, ethyl acetate was added, and stirred for a time to dissolve the precipitate, the phases were separated, the organic phase dried over Na2SO4 and the solvent evaporated. The crude product (934 mg) was purified by taking up in hexane/ethyl ether and filtered off to give 1.7 g of the title product.

1. temperaturewas refluxed for 6 hours
2. temperatureheated for an hour
3. temperatureheated for 3.5 hours
4. additionwas added
5. dissolutionto dissolve the precipitate
6. customthe phases were separated
7. dry with materialthe organic phase dried over Na2SO4
8. customthe solvent evaporated
9. customThe crude product (934 mg) was purified
10. filtrationfiltered off