HRID1967100

反应详情

EQUATION

反应方程式

HRID 1967100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 2,5-dibromo-3-thiophenecarboxylic acid (750 mg, 1.38 mmol)[prepared according to Goto, Hiromasa; Dai, Xiaoman; Narihiro, Harunori; Akagi, Kazuo Macromolecules 2004 37, 7, 2353-2362.] in dioxane/H2O (5:1, 6 mL) was added K2CO3 (486 mg, 3.52 mmol), tetrakistriphenylphosphine Pd(0) (51 mg, 44 umol), and 3-furanboronic acid (108 mg, 0.968 mmol). The reaction mixture was heated to 80° C. in a sealed tube. After 12 h, the solution was poured onto H2O (100 mL) and the pH was adjusted to ˜4 with aqueous HCl. The aqueous phase was extracted several times with DCM and the combined organic fractions were dried (Na2SO4), concentrated under vacuum and used directly: LC-MS (ES) m/z=273.

WORKUP

后处理

  1. additionthe solution was poured onto H2O (100 mL)
  2. extractionThe aqueous phase was extracted several times with DCM
  3. dry with materialthe combined organic fractions were dried (Na2SO4)
  4. concentrationconcentrated under vacuum