HRID578749

反应详情

EQUATION

反应方程式

HRID 578749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

[4-({[tert-Butyl(dimethyl)silyl]oxy}methyl)-3,5-difluorophenyl]boronic acid (19.3 g, 63.9 mmol; crude material, prepared by the method of Hattori, Bioorg. Med. Chem. 2006, 14, 3258-3262) was dissolved in 400 mL aqueous acetic acid (66%) and stirred at 40° C. for 5 h. The solution was then evaporated under reduced pressure, and the residue was purified by flash chromatography over silica gel (gradient elution from 0% to 2% methanol in dichloromethane) to give 3.46 g (25% of th., LC-MS purity 87%) of the title compound.

WORKUP

后处理

  1. customcrude material, prepared by the method of Hattori, Bioorg
  2. customThe solution was then evaporated under reduced pressure
  3. customthe residue was purified by flash chromatography over silica gel (gradient elution from 0% to 2% methanol in dichloromethane)