首页> 中文期刊> 《高等学校化学研究:英文版》 >Syntheses of 10-Hydroxy-5,10-dihydrophenophosphazine 10-Oxide and Its Methyl Derivatives

Syntheses of 10-Hydroxy-5,10-dihydrophenophosphazine 10-Oxide and Its Methyl Derivatives

         

摘要

Ph 2NH and PCl 3 interacted at a molar ratio of 1∶1 05 and slow elevated temperature and then at 210-220 ℃ for 6 h. The brown solution obtained was treated with H 2O to produce a very hard brown solid believed to be a mixture of 5,10 dihydrophenophosphazine 10 oxide(1a) and 10,10(5H,5H) spirobipenophosphazinium chloride(1b). This brown solid was directly oxidized with peracetic acid in HOAc prior to the separation of them to give compound 10 hydroxy 5,10 dihydropheno phosphazine 10 oxide(2) with a higher yield(45%) than that of the literature(27%). When treated with excess SOCl 2, compound 2 could quantitatively be converted to the corresponding phosphinyl chloride and the latter could further be transformed into 10 methoxy 5,10 dihydrophenophosphazine 10 oxide in 70% as treated with NaOMe in methanol. Compound 2 could also be converted to a bisanion when treated with NaH in DMF. The resulted bisanion reacted with MeI to give 5 methyl 10 hydroxy 5,10 dihydrophenophosphazine 10 oxide in a 73% yield which would be converted to 5 methyl 10 methoxy 5,10 dihydrophenophosphazine 10 oxide in a 56% yield by the same way of synthesizing 10 methoxy 5,10 dihydrophenophosphazine 10 oxide. All these compounds obtained were identified by surveying their melting points, and spectra and elemental analysis.
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