HRID1896032

反应详情

EQUATION

反应方程式

HRID 1896032 的结构方程式

PROCEDURE

实验过程

The title compound was prepared in the same way as the Compound of Example 274 but replacing Compound 274c with Compound 294a and 1-bromo-3,5-difluorobenzene with 3-iodofluorobenzene and adding 1 molar equivalent of tetrabutylammonium fluoride monohydrate to the starting reaction mixture. Purification by automated flash chromatography (Horizon™-Biotage) PE-EtOAc 100:30, then by CHCl3 followed by a final purification by preparative RP LC-MS chromatography, using MS-C18 XTerra column 30×50 mm eluting with ammonium bicarbonate 20 mM pH 8 buffer-acetonitrile gradient afforded a colourless oil. Yield: 20.4%. LCPREP. Colourless oil. Yield: 20.4%

WORKUP

后处理

  1. customto the starting reaction mixture
  2. customPurification by automated flash chromatography (Horizon™-Biotage) PE-EtOAc 100:30
  3. custompurification by preparative RP LC-MS chromatography
  4. washeluting with ammonium bicarbonate 20 mM pH 8 buffer-acetonitrile gradient
  5. customafforded a colourless oil