HRID746790

反应详情

EQUATION

反应方程式

HRID 746790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Heat in a sealed tube with stirring propane-2-sulfonic acid{2-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-thiophen-3-yl}-amide (0.5 mmol), 4-(4-Bromo-phenyl)-4-oxo-butyric acid (0.75 mmol), 2M Na2CO3 water solution (0.2 mL) and Pd(PPh3)4 (0.05 mmol) in 4.0 ml of an anhydrous DME to 100° C. for 24 h. Evaporate and purify the filtrate by flash chromotography (Silica gel-hexane/EtOAc). Add NaOH 2M (1 ml) to a suspension of the resultant ester (0.128 mmol) in ethanol (1 ml) and stir 24 h. Add 6N HCl until pH is approximately 1 and a white solid precipitates. Filter the solid to provide the title compound. MS (ES−): 456 (M−1).

WORKUP

后处理

  1. customEvaporate
  2. custompurify the filtrate by flash chromotography (Silica gel-hexane/EtOAc)
  3. customa white solid precipitates
  4. filtrationFilter the solid