反应详情

温度

100 °C

To a solution of methyl 2-bromo-3-cyclohexyl-1H-indole-6-carboxylate (from Example 1, Step 3) in dioxane (0.15 M) was added tri-n-butyl vinyl tin (1.1 eq.) followed by bis(triphenylphosphine)palladium(II) chloride (0.1 eq.). The reaction was stirred under nitrogen at 100° C. for 3 h and then cooled to RT. The mixture was then diluted with EtOAc and washed with brine (3×). The organic phase was then dried over Na2SO4 and evaporated to dryness. The residual material was purified by chromatography on silica gel (PE:EtOAc, 9:1). The product fractions were evaporated and the residual material re-crystallised from DCM with PE. The product was obtained as yellow crystalline material (60%).

1. temperaturecooled to RT
2. washwashed with brine (3×)
3. dry with materialThe organic phase was then dried over Na2SO4
4. customevaporated to dryness
5. customThe residual material was purified by chromatography on silica gel (PE:EtOAc, 9:1)
6. customThe product fractions were evaporated
7. customthe residual material re-crystallised from DCM with PE