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
- 60 °C
PROCEDURE
实验过程
To a solution of 5-[2-benzyloxy-4-(4-ethylpyridin-2-ylmethyl) -phenyl]-1,1-dioxo-2-(2-trimethylsilanyl-ethyl)-1,2,5-thiadiazolidin-3-one (47 mg, 0.088 mmol) in DMF (1 mL) is added CsF (80 mg, 0.53 mmol). The reaction is stirred at 60° C. for 2 h. The reaction is allowed to cool to ambient temperature and the solvent is evaporated under a stream of N2. The crude residue is taken up in acetonitrile and filtered, washing with acetonitrile several times. The solvent is removed under reduced pressure and the crude cesium salt of 5-[2-benzyloxy-4-(6-benzyloxypyridin-2-ylmethyl)-phenyl]-1,1-dioxo-1,2,5-thiadiazolidin-3-one is used in the next step without further purification: MS (M+H)+=516.
WORKUP
后处理
- temperatureto cool to ambient temperature
- customthe solvent is evaporated under a stream of N2
- filtrationfiltered
- washwashing with acetonitrile several times
- customThe solvent is removed under reduced pressure
- customthe crude cesium salt of 5-[2-benzyloxy-4-(6-benzyloxypyridin-2-ylmethyl)-phenyl]-1,1-dioxo-1,2,5-thiadiazolidin-3-one is used in the next step without further purification