反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionthe solution was poured onto H2O (100 mL)
- extractionThe aqueous phase was extracted several times with DCM
- dry with materialthe combined organic fractions were dried (Na2SO4)
- concentrationconcentrated under vacuum