反应详情

温度

100 °C

Tributylvinylstannane (1.15 eq.) and tetrakis(triphenylphosphine) palladium(0) (0.07 eq.) were added to a solution of compound 116 in toluene (0.09 M) and the reaction mixture was heated at 100° C. After 20 h volatiles were removed in vacuo and the residue was purified by column chromatography (SiO2, PE:EtOAc with EtOAc from 1 to 60%) to give a pale yellow solid, that was taken up in a 4N solution of HCl in dioxane (0.31 M). The reaction mixture was stirred for 1 h and the resulting white solid recovered by filtration, washed with EtOAc/petroleum ether affording the title compound 117 (99%) as a pale yellow solid. MS (ES+) m/z 405 (M+H)+.

1. customAfter 20 h volatiles were removed in vacuo
2. customthe residue was purified by column chromatography (SiO2, PE:EtOAc with EtOAc from 1 to 60%)
3. customto give a pale yellow solid, that
4. filtrationthe resulting white solid recovered by filtration
5. washwashed with EtOAc/petroleum ether affording the title compound 117 (99%) as a pale yellow solid