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
- 20 °C
PROCEDURE
实验过程
2.5 g (83 mmol) of sodium hydride (80% strength) and 17.6 g (80 mmol) of trimethylsulphoxonium iodide are initially introduced under a nitrogen atmosphere and 60 ml of absolute dimethyl sulphoxide are added dropwise at 10° C. The mixture is stirred for 1 hour at 20° C. and then 20 g (71 mmol) of 1-(4-chlorobenzoyl)-1-(3-chloro-1,2,4-triazol-1-yl)-cyclopropane dissolved in 30 ml of absolute dimethyl sulphoxide are added at 10° C. After 48 hours at 20° C., the mixture is warmed to 40° C. for 1 hour and the reaction solution is then poured into water. The mixture is extracted with ethyl acetate, the combined organic phases are washed with water and dried over sodium sulphate, and the solvent is evaporated in vacuo. 21 g of the title compound (100 % of theory) remain in the form of an oil.
WORKUP
后处理
- additionare added at 10° C
- waitAfter 48 hours at 20° C.
- temperaturethe mixture is warmed to 40° C. for 1 hour
- extractionThe mixture is extracted with ethyl acetate
- washthe combined organic phases are washed with water
- dry with materialdried over sodium sulphate
- customthe solvent is evaporated in vacuo