HRID2104945

反应详情

EQUATION

反应方程式

HRID 2104945 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-(tert-butyldimethylsilyloxy)-5-ethoxy-2-fluorobenzaldehyde (7.25 g, 24.3 mmol), prepared according to WO2003066588 A1, which is incorporated herein by reference, in 50 mL THF at 0° C., was added a 1 M solution of TBAF in THF (24.3 mL, 24.3 mmol). The mixture was stirred for 30 min, then was diluted with EtOAc, washed with H2O (2×) and brine, dried (Na2SO4) and concentrated. The crude product was purified by flash chromatography (0 to 50% EtOAc/hexanes gradient) to afford Intermediate 7.1, contaminated with tetrabutylammonium salts.

WORKUP

后处理

  1. washwashed with H2O (2×) and brine
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated
  4. customThe crude product was purified by flash chromatography (0 to 50% EtOAc/hexanes gradient)