HRID979457

反应详情

EQUATION

反应方程式

HRID 979457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

15.7 g (71.2 mmol) of trimethylsulphonium iodide are dissolved in 16 g of dimethyl sulphoxide under an atmosphere of nitrogen. 9.4 g (71.2 mmol) of potassium tert.-butylate are added at room temperature, with cooling. The mixture is allowed to stir for 6 hours and then a solution of 20 g (64.1 mmol) of 4-(2,4-dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butanone in 30 ml of tetrahydrofuran is added. The reaction mixture is allowed to stir at room temperature for 15 hours and under reflux for 4 hours, then cooled and poured into water. The mixture is extracted with methylene chloride, and the organic phase is dried over sodium sulphate and evaporated in vacuo. 15.4 g (73.7% of theory) of 2-(2,4-dichlorophenyl-tert.-butyl)-2-(1,2,4-triazol-1-ylmethyl)oxirane of refractive index nD20 =1.5539 are obtained. ##STR95##

WORKUP

后处理

  1. temperaturewith cooling
  2. stirringto stir at room temperature for 15 hours
  3. temperatureunder reflux for 4 hours
  4. temperaturecooled
  5. extractionThe mixture is extracted with methylene chloride
  6. dry with materialthe organic phase is dried over sodium sulphate
  7. customevaporated in vacuo