反应详情

2-Chlorophenylisocyanate (7 g) and trimethylsilyl azide (7.9 g) were mixed and heated under refluxing for eight hours. The excessive trimethylsilyl azide was distilled off under reduced pressure and to the residue there were added 40 ml of methanol. Thereafter, the methanol was evaporated and the residue was purified by flush column chlomatography (hexane:ethyl acetate=2:1) to obtain the desired 1-(2-chlorophenyl)-5(4H)-tetrazolinone (7 g) having a melting point in the range of from 124.5° to 125.5° C.

1. temperatureheated
2. temperatureunder refluxing for eight hours
3. distillationThe excessive trimethylsilyl azide was distilled off under reduced pressure and to the residue there
4. additionwere added 40 ml of methanol
5. customThereafter, the methanol was evaporated
6. customthe residue was purified
7. customby flush column chlomatography (hexane:ethyl acetate=2:1)