《A New Technique of Synthesizing 10-Hydroxy-5-methyl- 5,10- dihydrophenophosphazine 10-Oxide》.pdfVIP

Chinese Chemical Letters Vol. 14, No. 4, pp 347 – 350, 2003 347 /journal/ccl.html A New Technique of Synthesizing 10-Hydroxy-5-methyl- 5,10- dihydrophenophosphazine 10-Oxide 1,2 1 Zhi Gang YIN , De Feng ZHAO * 1State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116012 2 Chemical Engineering Department, Zhengzhou Institute of Light Industry, Zhengzhou 450002 Abstract: 10-Hydroxy-5-methyl-5, 10- dihydrophenophosphazine 10-oxide (1) was prepared by a new technique of treating 10-methoxy-5,10-dihydrophenophosphazine 10-oxide (2) with an equivalent of NaH in anhydrous DMF, and then at 120C for 3~4 h, which not only avoided poisonous and expensive methyl iodide used in literature, but made the consumption of NaH greatly decrease as well. The possible reaction mechanism was also described. The chemical structure of 1 was confirmed by IR, NMR, and mass spectroscopy. Keywords : 10-Dihydrophenophosphazine, synthesis, structure identification. The amino derivatives of title compound 1 are nonmutagenic intermediates1 which are potential substitute for strong carcinogenic intermediates of -naphthylamine and benzidine residue in some well-known carcinogenic -naphthylamine- and benzidine- based azo dyes which are now