HRID1704639

反应详情

EQUATION

反应方程式

HRID 1704639 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Methyl-1,2,5-thiadiazole-3-one (11.6 g., 0.1 mole) was dissolved in dry methylene chloride (100 ml.) and under a nitrogen atmosphere was added methyl fluorosulfonate (8.2 ml., 0.1 mole) and the reaction mixture was stirred at room temperature for 1 hour. Further, methyl fluorosulfonate (0.1 ml.) was added and the reaction continued at reflux for one further hour. The reaction was cooled, the precipitate separated by filtration and washed with several portions of cold methylene chloride. Yield 13 g. The compound was stored in a dry atmosphere, m.p., 138°-139° C.

WORKUP

后处理

  1. temperatureat reflux for one further hour
  2. temperatureThe reaction was cooled
  3. customthe precipitate separated by filtration
  4. washwashed with several portions of cold methylene chloride
  5. customwas stored in a dry atmosphere, m.p., 138°-139° C.