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
- 25 °C
PROCEDURE
实验过程
To a stirred solution of 3-[(hydroxyimino)(1-methyl-1H-tetrazol-5-yl)methyl]-N,N-dimethylaniline (1.25 g, 5.07 mmol) in acetonitrile (50 mL), were added cesium carbonate (3.47 g, 10.6 mmol), potassium iodide (421 mg, 2.53 mmol) and 2-bromo-4-bromomethyl-thiazole (1.44 g, 5.58 mmol). The resulting suspension was stirred at 25° C. for 4 h and 30 minutes. After cooling, the suspension was filtered, the filtrate was diluted with ethyl acetate (250 mL), washed with water (2×100 mL), dried over MgSO4 and concentrated in vacuo. Purification on silica gel afforded 3-[{[(2-bromo-1,3-thiazol-4-yl)methoxy]imino}(1-methyl-1H-tetrazol-5-yl)methyl]-N,N-dimethylaniline as an oil [1.83 g, yield 86%;
WORKUP
后处理
- temperatureAfter cooling
- filtrationthe suspension was filtered
- additionthe filtrate was diluted with ethyl acetate (250 mL)
- washwashed with water (2×100 mL)
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customPurification on silica gel