HRID2426667

反应详情

EQUATION

反应方程式

HRID 2426667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureThe solution was heated at 100° C. overnight
  2. concentrationThe reaction mixture was then concentrated in vacuo, and water/ethyl acetate
  3. additionwere added to the residue
  4. extractionThe aqueous phase was extracted three times with ethyl acetate
  5. dry with materialdried over sodium sulfate
  6. customthe solvent was removed in vacuo
  7. custompurified by preparative HPLC