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