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
Under a nitrogen atmosphere, methyl N-(t-butyloxycarbonyl)-2-amino-2-(4-toluenesulfonyloxyphenyl)acetate (0.44 g, 1.0 mmol), cesium carbonate (0.65 g, 2.0 mmol), tricyclohexylphosphine (0.059 g, 0.2 mmol), bis(1,5-cyclooctadiene)nickel (0.028 g, 0.1 mmol) and 2,6-dimethoxyphenylboronic acid (0.36 g, 2.0 mmol) were mixed in dioxane (1 ml). The reaction mixture was heated to 70° C. and then stirred at the same temperature for 9 hrs. After the reaction was completed, the mixture was left to cool to room temperature and insoluble substances were filtered off. The filtrate was subjected to column chromatography purification to obtain methyl N-(t-butyloxycarbonyl)-2-amino-2-[4-(2,6-dimethoxyphenyl)phenyl]acetate (0.29 g, yield 72%) as pale yellow oil.
WORKUP
后处理
- waitthe mixture was left
- temperatureto cool to room temperature
- filtrationinsoluble substances were filtered off
- customThe filtrate was subjected to column chromatography purification