HRID1645828

反应详情

EQUATION

反应方程式

HRID 1645828 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The 5-acetonylthio-1-methyltetrazole, prepared as above described, was dissolved in 20 ml of methylene chloride and to the resulting solution was added 0.617 gram (0.0055 mol) of methyl trifluoromethanesulfonate and the mixture allowed to stand overnight at room temperature. Thereafter, the solvent was vaporized off and an oily residue obtained. The latter was dissolved in aqueous methanol and the methanol solution passed over a Dowex-1 (Cl-) ion exchange column. The eluate from the column was evaporated to obtain a waxy material which was triturated with hexane to obtain a waxy solid which after drying in high vacuum amounted to 0.80 gram of 5-acetonylthio-1,4-dimethyltetrazolium chloride, m.p. 102°-104° C.

WORKUP

后处理

  1. customan oily residue obtained
  2. customThe eluate from the column was evaporated
  3. customto obtain a waxy material which
  4. customwas triturated with hexane
  5. customto obtain a waxy solid which
  6. customafter drying in high vacuum