HRID728031

反应详情

EQUATION

反应方程式

HRID 728031 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3.12 g (0.02 mol) of 5-mercapto-1-methyltetrazole sodium salt hydrate in 60 ml of absolute ethanol was added dropwise, 2.06 g (0.2 mol) of chloroacetone. After stirring for 20 hours at room temperature, the ethanol was evaporated in vacuo. The residue was dissolved in methylene chloride and was washed with water and then brine prior to drying over Na2SO4. Evaporation of the methylene chloride solution gave 1-methyl-5-acetonylthiotetrazole that was purified by flash chromatography on silica gel to yield 0.94 g of the 5-acetonylthio-1-methyltetrazole product.

WORKUP

后处理

  1. customthe ethanol was evaporated in vacuo
  2. dissolutionThe residue was dissolved in methylene chloride
  3. washwas washed with water
  4. dry with materialbrine prior to drying over Na2SO4
  5. customEvaporation of the methylene chloride solution