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 120...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.展开更多
The title compound (1) was treated with NaH at room temperature in anhydrous DMF to give a sodium salt (containing nitrogen anion) which could shift the methyl group from oxygen to nitrogen atom to form N-methyl phosp...The title compound (1) was treated with NaH at room temperature in anhydrous DMF to give a sodium salt (containing nitrogen anion) which could shift the methyl group from oxygen to nitrogen atom to form N-methyl phosphinic acid as the reaction temperature was increased to 120 ℃. Three nitro derivatives containing 5,10-dihydrophenophosphazine ring system were prepared for the investigation on the above reaction mechanism which would be possibly regarded as a special inter-molecular substitution, viz., the nucleophilic nitrogen anion from one molecule of 1 attacked the carbon atom of the O-methyl of another 1. In addition, the chemical structures of seven compounds containing 5,10-dihydrophenophos-phazine ring system involved in the experiment were confirmed by IR, 1H NMR, 31P NMR and mass spectroscopy.展开更多
基金The authors would like to acknowledge support from the National Natural Science Foundation of China(29972006) especially to express the deep appreciation to Professor Q. J. Peng and Miss K. Jin from our laboratory for their assistance in performing str
文摘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.
基金ProjectsupportedbytheNationalNaturalScienceFoundationofChina (No .2 9972 0 0 6)
文摘The title compound (1) was treated with NaH at room temperature in anhydrous DMF to give a sodium salt (containing nitrogen anion) which could shift the methyl group from oxygen to nitrogen atom to form N-methyl phosphinic acid as the reaction temperature was increased to 120 ℃. Three nitro derivatives containing 5,10-dihydrophenophosphazine ring system were prepared for the investigation on the above reaction mechanism which would be possibly regarded as a special inter-molecular substitution, viz., the nucleophilic nitrogen anion from one molecule of 1 attacked the carbon atom of the O-methyl of another 1. In addition, the chemical structures of seven compounds containing 5,10-dihydrophenophos-phazine ring system involved in the experiment were confirmed by IR, 1H NMR, 31P NMR and mass spectroscopy.
