An efficient and rapid detosylation of N,N',N", A'""-tetra(p-tosyl)- 1,4,7,10-tetraazacyclododecane, the key intermediates in Atikins' route for preparing 1,4,7,10-tetraazacyclododecane, has been investigated by hydrolysis in concentrated sulfuric acid under microwave irradiation condition in a simply refitted domestic microwave oven equipped with an electromagnetic stirrer and a refluxing condenser. The results indicated that the hydrolysis and detosylation of poly(p-tosyl) compounds were completed within 50～120 s in 95%～98% sulfuric acid under the irradiation power of 75～375 W. In comparison with the common hydrolysis which was completed for 2～3 d at 14℃ in 96%～98% sulfuric acid, the microwave irradiation accelerated (MIA) hydrolysis is rather rapid.

Key words: NITROGEN HETEROCYCLICS, p-tolunosulfamide, HYDROLYSIS, ACYLATION