HRID1670097

反应详情

EQUATION

反应方程式

HRID 1670097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

3-Bromo-5-{6-[2-(2-ethoxycarbonyl-ethyl)-3-(3-ethoxycarbonyl-propoxy)-phenyl]-hexyloxy}-benzoic acid tert-butyl ester (2.0 g) was dissolved in 1,2-dimethoxyethane (40 mL), followed by addition of Pd(PPh3)4 (80 mg), 2 M solution of sodium carbonate (6 mL) and 4-methyl-3-thiopheneboronic acid (641 mg). The resulting reaction mixture was stirred at 85° C. for 2 h. After cooling the reaction mixture was filtered through Celite™, diluted with ethyl acetate and washed with water and brine. The organic extract was dried over anhydrous sodium sulfate, concentrated under reduced pressure and purified on a silica gel column using ethyl acetate and hexanes to the title compound (1.8 g, 88% yield).

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. temperatureAfter cooling the reaction mixture
  3. filtrationwas filtered through Celite™
  4. additiondiluted with ethyl acetate
  5. washwashed with water and brine
  6. extractionThe organic extract
  7. dry with materialwas dried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. custompurified on a silica gel column