反应 #41329

反应方程式

2,2,2-trifluoro-N-((1R,2S)-1-(1-(4-fluorophenyl)-1H-indazol-5-yloxy)-1-(3-methoxyphenyl)propan-2-yl)acetamide

2,2,2-Trifluoro-N-[(1R,2S)-1-[1-(4-fluorophenyl)indazol-5-yl]oxy-1-(3-methoxyphenyl)propan-2-yl]acetamide

aluminium chloride

→

product

收率 42.2%

2,2,2-Trifluoro-N-[(1R,2S)-1-[1-(4-fluorophenyl)indazol-5-yl]oxy-1-(3-hydroxyphenyl)propan-2-yl]acetamide

收率 42.2%

溶剂

methylbenzene

反应条件

后处理

1. 1
   其他Methylbenzene was removed in vacuo
2. 2
   workup.ADDITIONthe solution in dodecanethiole was diluted with n-heptane (10 ml)
3. 3
   其他Oily precipitate has formed
4. 4
   洗涤which was washed with heptane
5. 5
   其他dried in vacuo
6. 6
   workup.DISSOLUTIONdissolved in acetonitrile/water mixture
7. 7
   其他The crude product was purified by preparative HPLC

实验过程

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 aluminium 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%).

来源