HRID1174980

反应详情

EQUATION

反应方程式

HRID 1174980 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 2,4-dichlorophenyl boronic acid (3.96 g, 15.11 mmol) and 4-Iodo-benzoic acid methyl ester (2.88 g, 15.11 mmol), K2CO3 (7.31 g, 52.89 mmol) in 1,4-dioxane (85 mL), and water (20 mL) is purged with nitrogen for 10 min. Pd(PPh3)4 (0.87 g, 0.756 mmol) is added and the resulting reaction mixture is refluxed overnight. The reaction is diluted with water and extracted with Et2O. The combined organic layers are washed with water, dried with MgSO4, and concentrated. The crude material is purified by chromatography to give the title compound (2.20 g, 50%). LC/MS (m/z): calcd for C13H18Cl2O2: 267.1; found: 266.9.

WORKUP

后处理

  1. customthe resulting reaction mixture
  2. temperatureis refluxed overnight
  3. extractionextracted with Et2O
  4. washThe combined organic layers are washed with water
  5. dry with materialdried with MgSO4
  6. concentrationconcentrated
  7. customThe crude material is purified by chromatography