HRID1461804

反应详情

EQUATION

反应方程式

HRID 1461804 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-amino-6-fluoro-3-(5-methyl-1,2,4-oxadiazol-3-ylmethyl)-2(3H)-benzothiazolone (1.33 g) and dioxane (23 g) was prepared. To this mixture was dropwise added trichloromethyl chloroformate (1 g). The reaction mixture was heated under refluxing for 3 hours. The components with lower boiling points were distilled off, and the residue was dissolved in toluene (50 ml). The resulting solution was concentrated under a reduced pressure to dryness, so that the aimed compound, i.e. 6-fluoro-5-isocyanato-3-(5-methyl-1,2,4-oxadiazol-3-ylmethyl)-2(3H)-benzothiazolone (1.46 g) was obtained. m.p. 125°-127° C.

WORKUP

后处理

  1. customwas prepared
  2. temperatureThe reaction mixture was heated
  3. temperatureunder refluxing for 3 hours
  4. distillationThe components with lower boiling points were distilled off
  5. dissolutionthe residue was dissolved in toluene (50 ml)
  6. concentrationThe resulting solution was concentrated under a reduced pressure to dryness, so that the aimed compound