反应详情

温度

100 °C

132 g (408 mmol) of the compound from Example 59A (alternative synthesis) are dissolved in 1.27 l of anhydrous dioxane, 136 g (428 mmol) of tributylvinyltin and 9.44 g (8.17 mmol) of tetrakis(triphenylphosphine)palladium are added and the mixture is stirred at 100° C. for 4 h. The mixture is allowed to cool and filtered through kieselguhr. The mixture is concentrated to dryness under reduced pressure. The residue is dissolved in dichloromethane and purified by chromatography on silica gel (petroleum ether/ethyl acetate 9:1, then 8:2, then 7:3). The product-containing fractions are combined, the solvents are removed and the residue is triturated with petroleum ether/diethyl ether (10:1). This gives 83 g (75% of theory) of the desired product.

1. temperatureto cool
2. filtrationfiltered through kieselguhr
3. concentrationThe mixture is concentrated to dryness under reduced pressure
4. dissolutionThe residue is dissolved in dichloromethane
5. custompurified by chromatography on silica gel (petroleum ether/ethyl acetate 9:1
6. customthe solvents are removed
7. customthe residue is triturated with petroleum ether/diethyl ether (10:1)