HRID751021

反应详情

EQUATION

反应方程式

HRID 751021 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A methanol/dioxane (20 mL/5 mL of methanol/dioxane) solution/suspension of 4-iodo-3-nitrothioanisole (1 mmol), Pd(OAc)2 (0.01 mmol) was purged with argon for ˜5 min. To this solution Et3N (3 mmol), and 5 mL of water were added and purged with argon for another 5 min. To the above solution, 2-aminophenyl boronic acid (2 mmol, solution in 5 mL of DMF, purged with argon), was added and the reaction mixture was heated at 70° C. (oil bath temperature) for 2 h. The reaction was monitored by HPLC and LC-MS to follow the product formation. The reaction mixture was then cooled down to room temperature and filtered through diatomaceous earth. The filtrate was concentrated and purified using preparative HPLC.

WORKUP

后处理

  1. customwas purged with argon for ˜5 min
  2. custompurged with argon for another 5 min
  3. temperatureThe reaction mixture was then cooled down to room temperature
  4. filtrationfiltered through diatomaceous earth
  5. concentrationThe filtrate was concentrated
  6. custompurified