反应详情

温度

175 °C

Under Ar, a solution of the product from Example 100 (53.2 mg, 172 mol) in 1,4-dioxane (1 ml) and toluene (1.5 ml) was treated with Tris(dibenzylidene-acetone)dipalladium (15 mg, 17 mol), racemic-2,2′-Bis(diphenylphosphino)-1,1′-binaphthyl (20 mg, 34 mol), 4-methoxybenzenethiol (26 l, 206 mol), and sodium tert-butoxide (23.5 mg, 241 mol). This mixture was then heated to 175° C. by microwave for 1 h. After cooled to ambient temperture, the reaction mixture was diluted with ethyl acetate (30 ml) and methanol (30 ml), filtered though a celite pad and then the filtrate was concentrated in vacuo. The residue was purified with flash chromatography (hexanes/ethyl acetate 2:1), to afford the title compound, (35.6 mg, 56%); MS (ES+) m/e 369 [M+H]+.

1. temperatureAfter cooled to ambient temperture
2. filtrationfiltered though a celite pad
3. concentrationthe filtrate was concentrated in vacuo
4. customThe residue was purified with flash chromatography (hexanes/ethyl acetate 2:1)