HRID1461804
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customwas prepared
- temperatureThe reaction mixture was heated
- temperatureunder refluxing for 3 hours
- distillationThe components with lower boiling points were distilled off
- dissolutionthe residue was dissolved in toluene (50 ml)
- concentrationThe resulting solution was concentrated under a reduced pressure to dryness, so that the aimed compound