HRID1258603

反应详情

EQUATION

反应方程式

HRID 1258603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureAfter cooling
  2. filtrationthe suspension was filtered
  3. additionthe filtrate was diluted with ethyl acetate (250 mL)
  4. washwashed with water (2×100 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. customPurification on silica gel