反应详情

温度

175 °C

Under Ar, a solution of the product from Example 100 (24 mg, 77.6 mol) in 1,4-dioxane (0.8 ml) and toluene (1.2 ml) was treated with Tris(dibenzylidene-acetone)dipalladium (7.2 mg, 7.8 mol), racemic-2,2′-Bis(diphenylphosphino)-1,1′-binaphthyl (9.7 mg, 15.6 mol), aniline (8.5 l, 93.1 mol), and sodium tert-butoxide (10.5 mg, 108.6 mol). This mixture was then heated to 175° C. by microwave for 45 min. After cooled to ambient temperture, the reaction mixture was diluted with ethyl acetate (30 ml), filtered though a celite pad and then the filtrate was concentrated in vacuo. The residue was purified with reverse phase HPLC (10% MeCN/H2O→80% MeCN/H2O), to afford the title compound, (6.3 mg, 24%); MS (ES+) m/e 322 [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 reverse phase HPLC (10% MeCN/H2O→80% MeCN/H2O)