HRID628502

反应详情

EQUATION

反应方程式

HRID 628502 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(2-methyl-3-triisopropylsilanylsulfanylphenyl)-4-methyl-1,4-dihydrotetrazole-5-one 3.63 g, cesium fluoride 2.91 g and N,N-dimethylformamide 10 ml was stirred at room temperature for thirty minutes. To the resulting mixture was added methyl iodide 2.72 g and the resulting mixture was stirred at room temperature for three hours. To the reaction mixture was added water and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated saline, and was dried over anhydrous magnesium sulfate and was then concentrated under reduced pressure. The resulting residue was subjected to a silica gel column chromatography to give 1-(2-methyl-3-methylthiophenyl)-4-methyl-1,4-dihydrotetrazole-5-one 1.65 g.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred at room temperature for three hours
  2. extractionthe resulting mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated saline
  4. dry with materialwas dried over anhydrous magnesium sulfate
  5. concentrationwas then concentrated under reduced pressure