反应详情

温度

40 °C

To a stirred solution of 2,2,2-trifluoro-N-((1R,2S)-1-(1-(4-fluorophenyl)-1H-indazol-5-yloxy)-1-(3-methoxyphenyl)propan-2-yl)acetamide (Example 6, 10 mg, 20 μmol) in methylbenzene (1 ml) was added dodecanethiole (1 ml), followed with anhydrous aluminum chloride (5.3 mg, 40 μmol). The mixture was stirred at 40° C. for 1 h. Methylbenzene was removed in vacuo, the solution in dodecanethiole was diluted with n-heptane (10 ml). Oily precipitate has formed, which was washed with heptane, dried in vacuo, and dissolved in acetonitrile/water mixture. The crude product was purified by preparative HPLC afforded 4 mg of product as a white solid (42%).

1. customMethylbenzene was removed in vacuo
2. additionthe solution in dodecanethiole was diluted with n-heptane (10 ml)
3. customOily precipitate has formed
4. washwhich was washed with heptane
5. customdried in vacuo
6. dissolutiondissolved in acetonitrile/water mixture
7. customThe crude product was purified by preparative HPLC