HRID1085800

反应详情

EQUATION

反应方程式

HRID 1085800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9.6 g (0.044 mole) of trimethylsulphonium iodide are dissolved in 9.6 g (0.118 mole) of dimethyl sulphate under a nitrogen atmosphere. 5.2 g (0.044 mole) of potassium tert.-butylate are added at room temperature and the mixture is subsequently stirred at room temperature for 6 hours. A solution of 9.9 g (0.0397 mole) of 4-chlorophenyl 2-(1,2,4-triazol-1-yl)-prop-2-yl ketone in 16 ml of tetrahydrofuran is then added dropwise at room temperature. The reaction mixture is subsequently led at room temperature for 15 hours and under reflux for 4 hours, cooled and filtered. The filtrate is concentrated in vacuo, the residue is discharged onto water and the mixture is extracted with methylene chloride. The organic phase is dried over sodium sulphate and concentrated in vacuo. 10.4 g (100% of theory) of 2-(4-chlorophenyl-2-[2-(1,2,4-triazol-1-yl)-prop-2-yl]-oxirane of refractive indes nD20 1.5388 are obtained. ##STR18##

WORKUP

后处理

  1. waitThe reaction mixture is subsequently led at room temperature for 15 hours
  2. temperatureunder reflux for 4 hours
  3. temperaturecooled
  4. filtrationfiltered
  5. concentrationThe filtrate is concentrated in vacuo
  6. extractionthe mixture is extracted with methylene chloride
  7. dry with materialThe organic phase is dried over sodium sulphate
  8. concentrationconcentrated in vacuo