HRID878212

反应详情

EQUATION

反应方程式

HRID 878212 的结构方程式

PROCEDURE

实验过程

The title compound was prepared in analogy to example 90, from [4-(4-fluoro-2-methoxy-phenyl)-pyridin-3-yl]-(2-methanesulfonyl-ethyl)-amine (example 162, intermediate) and 3,5-bis(trifluoromethyl)benzoic acid (CAS RN 725-89-3) after a reaction time of 40 hours. The compound was purified by silica gel chromatography using a MPLC system (ISCO) and a 10 g and 5 g column, respectively, eluting with a gradient of n-heptane:EtOAc (100:0 to 0:100). A third chromatography, using preparative HPLC (Gemini NX column) eluting with a gradient of methanol:water (containing 0.05% formic acid) (20:80 to 98:2), yielded the product as a colorless solid (4%). MS (ESI): m/z=565.10 [M+H]+.

WORKUP

后处理

  1. customThe compound was purified by silica gel chromatography
  2. washa 10 g and 5 g column, respectively, eluting with a gradient of n-heptane:EtOAc (100:0 to 0:100)
  3. washeluting with a gradient of methanol