HRID1835451

反应详情

EQUATION

反应方程式

HRID 1835451 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a suspension of 2-bromo-5-methoxycarbonylthiophene (1.11 g) and phenylboronic acid (0.79 g) and tetrakis(triphenylphosphine)-palladium (289 mg) in 1,2-dimethoxyethane (10 ml) was added an aqueous solution of sodium carbonate (2M, 6.5 ml) followed by stirring at 80° C. for 18 hours. The mixture was diluted with dichloromethane and washed with water and brine. The mixture was dried over magnesium sulfate and evaporated under reduced pressure. The residue was triturated with methanol. The resulting precipitate was collected by filtration, washed with methanol and diisopropyl ether and dried to give 2-methoxycarbonyl-5-phenylthiophene (918 mg, 84.2%).

WORKUP

后处理

  1. washwashed with water and brine
  2. dry with materialThe mixture was dried over magnesium sulfate
  3. customevaporated under reduced pressure
  4. customThe residue was triturated with methanol
  5. filtrationThe resulting precipitate was collected by filtration
  6. washwashed with methanol and diisopropyl ether
  7. customdried