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Phosphates 및 Phosphoric Amides의 합성 (제1보)
최길영,최삼권,Kil-Yeong Choi,Sam-Kwon Choi 대한화학회 1980 대한화학회지 Vol.24 No.6
Phosphoryl chloride와 allyl alcohol, 2,3-dibromopropanol, 2-pyrrolidone, ethylenimine을 반응하여 여러가지 phosphate와 phospshoric amide를 합성하였다. 합성한 화합물은 모두 열에 불안정하였으며, allyl phosphorodichloridate와 diallyl phosphorochloridate는 증류하면 상당량의 중합체가 생겼다. IR 스펙트라에서는 $1,300∼1,200 cm^{-1}$에서 P=O stretching의 특성밴드가 나타났으며 NMR 스펙트라는 인원자의 long range coupling 효과로 인해 복잡한 피이크를 보였다. 2,3-dibromopropyl phosphordichloridate의 mass 스펙트럼에서는 분자이온 피이크를 볼 수 없었다. Phosphates and phosphoric amides were synthesized by the reaction of phosphoryl chloride with allyl alcohol, 2,3-dibromopropanol, 2-pyrrolidone and ethylenimine. All of these compounds were thermally very unstable. Allyl phosphorodichoridate and diallyl phosphorochloridate gave significant amount of polymeric products when they were distilled. IR spectra showed characteristic P=O stretching bands between 1300 and $1200 cm^{-1}$ and NMR spectra were very complicated due to the long range coupling effect of phosphorus atom. And mass spectrum of 2,3-dibromopropyl phosphorodichloridate gave no indication of molecular ion peak.
Phosphates 및 Phosphoric Amides의 합성 (제2보)
최길영,최삼권,Kil-Yeong Choi,Sam-Kwon Choi 대한화학회 1980 대한화학회지 Vol.24 No.6
Tris(hydroxyethyl) phosphate, ethylphosphoramidic dichloride, N,N-diethylphosphoramidic dichloride, bis(hydroxyethyl) N-ethylphosphoramidate 나 bis(hydroxyethyl) N,N-diethylphosphoramidate를 합성하고 특성을 고찰하였다. Phosphate와 두종류의 phosphoramidate는 감압하에서 가열하면 ethylene glycol이 빠지면서 중합반응이 일어났으며 이들 화합물의 mass 스펙트라에서는 분자이온피이크를 관찰할 수 없었다. 또한 ethylphosphoramidic dichloride도 180$^{\circ}C$에서 HCl이 발생되면서 중합체로 변하였다. IR스펙트라에서는 P=O strectching의 특성밴드가 $1,300{\sim}1,200 cm^{-1}$에서 나타났다. Tris(hydroxyethyl) phosphate, ethylphosphoramidic dichloride, N,N-diethylphosphoramidic dichloride, bis(hydroxyethyl) N-ethylphosphoramidate and bis(hydroxyethyl) N,N-diethylphosphoramidate were synthesized and characterized. Phosphate and phosphoramidates were polymerized with the elimination of ethylene glycol when heated under reduced pressure and they gave no molecular ion peaks in their mass spectra. And also ethylphosphoramidic dichloride gave polymeric products at 180$^{\circ}C$ with the evolution of HCl. IR spectra showed characteristic P=O streching bands in the range of 1,300 to$ 1,200 cm^{-1}.$