HRID2426667
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
PROCEDURE
实验过程
0.009 g of Pd(PPh3)4 was added to a solution of 0.091 g of ethyl 4-iodobenzoate in 0.96 ml of degassed toluene and stirred at room temperature for 10 minutes. Then a solution of 0.047 g of 2,4-difluorophenylboronic acid in 0.114 ml of ethanol and 0.201 ml of a 2N Na2CO3 solution was added to the reaction solution. The solution was heated at 100° C. overnight. The reaction mixture was then concentrated in vacuo, and water/ethyl acetate were added to the residue. The aqueous phase was extracted three times with ethyl acetate and dried over sodium sulfate, and the solvent was removed in vacuo and purified by preparative HPLC.
WORKUP
后处理
- temperatureThe solution was heated at 100° C. overnight
- concentrationThe reaction mixture was then concentrated in vacuo, and water/ethyl acetate
- additionwere added to the residue
- extractionThe aqueous phase was extracted three times with ethyl acetate
- dry with materialdried over sodium sulfate
- customthe solvent was removed in vacuo
- custompurified by preparative HPLC