The title compound, 2-（3-silatranylpropylamino）-4-dichlorophenyl-5,5-dimethyl- 1,3,2-dioxaphosphorinane-2-oxide （2（C20H33N2O6Psi）？C2H6O？CH4O, Mr = 991.20）, has been synthe- sized by the nucleophilic substituti...The title compound, 2-（3-silatranylpropylamino）-4-dichlorophenyl-5,5-dimethyl- 1,3,2-dioxaphosphorinane-2-oxide （2（C20H33N2O6Psi）？C2H6O？CH4O, Mr = 991.20）, has been synthe- sized by the nucleophilic substitution reaction of 2-chloro-4-phenyl-5,5-dimethyl-1,3,2-dioxa- phosphorinane-2-oxide with γ-aminopropylsilatrane, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P with a = 10.3783（15）, b = 11.2402（17）, c = 12.1675（18） ？, ？ = 70.653（4）, ？ = 82.908（4）, ？ = 85.690（4）？, V = 1328.1（3） ？3, Z = 1, Dc = 1.239 g/cm3, μ = 0.19 mm？1, F（000） = 532, the final R = 0.0640 and wR = 0.2090 for 3615 observed reflections with I 〉 2？（I）. The cyclic dioxaphosphorinane ring in the molecule adopts a thermodynamically stable cis conformation, while the silatrane fragment forms a cage-like structure in which there exists an intramolecular Si？N donor-acceptor bond. In the crystal structure, centrosymmetrically related molecules are linked by pairs of N–H？？？O hydrogen bonds into dimers, generating rings with graph-set motif R22（8）. Furthermore, a couple of O（7）–H（10）？？？O（3） hydrogen bonds were formed by O atom of P=O and H atom from hydroxyl in the solvent ethanol. Thermal property of the compound was also studied by means of thermogravimetry （TGA）. The thermal analysis and preliminary fireproofing test show that the title compound has good flame retardance.展开更多
A novel polyester containing glycolic acid(GA)and 2 hydro 2 oxo 1,3,2 dioxaphosphorinane(TMP)was prepared by ring opening polymerization.The composition and the structure of the titled polymer were investigated by 1...A novel polyester containing glycolic acid(GA)and 2 hydro 2 oxo 1,3,2 dioxaphosphorinane(TMP)was prepared by ring opening polymerization.The composition and the structure of the titled polymer were investigated by 1H NMR, 13 C NMR,FT IR,EA,and VPO.The influence of time on total conversion and molecular weight was also studied.展开更多
The stereoselective synthesis of 2-chloro-4-substituted-phenyl-5,5-dimethyl-1,3,2-dioxaphosphorinan-2-(thi)ones is described. Only single trans-isomers were obtained when 1-substituted-phenyl-2,2-dimethyl-1,3-propaned...The stereoselective synthesis of 2-chloro-4-substituted-phenyl-5,5-dimethyl-1,3,2-dioxaphosphorinan-2-(thi)ones is described. Only single trans-isomers were obtained when 1-substituted-phenyl-2,2-dimethyl-1,3-propanediols (1) reacted with POCl3. But the stereoselectivity of cyclization reaction between (1) and PSCl3 depended greatly upon the reaction condition. The configurational assignments and the ratio of cis-/trans- diastereoisomers of the products were performed on the basis of (HNMR)-H-1, (PNMR)-P-31 and IR spectra and confirmed by X-ray diffraction analyses.展开更多
In order to construct the zwitterionic structure of phosphorylcholine onto the surface of biomaterials, five novel phospholanes containing hydroxyl group were synthesized from the corresponding diol and 2-chloro-2-oxo...In order to construct the zwitterionic structure of phosphorylcholine onto the surface of biomaterials, five novel phospholanes containing hydroxyl group were synthesized from the corresponding diol and 2-chloro-2-oxo-1,3,2-dioxaphospholane in the presence of THF. Then, five novel phosphorylcholines containing hydroxyl group were prepared by the corresponding phospholane and anhydrous trimethylamine in the presence of acetonitrile. Their structures were characterized by FTIR, 1H NMR and elemental analysis.展开更多
基金Supported by the Youth Foundation of Hubei Educational Committee(No.Q20151902)the State Undergraduate Innovative Training Program(No.201410517002)the Start-up Foundation for Doctor of Hubei University for Nationalities(No.MY2013B027)
文摘The title compound, 2-（3-silatranylpropylamino）-4-dichlorophenyl-5,5-dimethyl- 1,3,2-dioxaphosphorinane-2-oxide （2（C20H33N2O6Psi）？C2H6O？CH4O, Mr = 991.20）, has been synthe- sized by the nucleophilic substitution reaction of 2-chloro-4-phenyl-5,5-dimethyl-1,3,2-dioxa- phosphorinane-2-oxide with γ-aminopropylsilatrane, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P with a = 10.3783（15）, b = 11.2402（17）, c = 12.1675（18） ？, ？ = 70.653（4）, ？ = 82.908（4）, ？ = 85.690（4）？, V = 1328.1（3） ？3, Z = 1, Dc = 1.239 g/cm3, μ = 0.19 mm？1, F（000） = 532, the final R = 0.0640 and wR = 0.2090 for 3615 observed reflections with I 〉 2？（I）. The cyclic dioxaphosphorinane ring in the molecule adopts a thermodynamically stable cis conformation, while the silatrane fragment forms a cage-like structure in which there exists an intramolecular Si？N donor-acceptor bond. In the crystal structure, centrosymmetrically related molecules are linked by pairs of N–H？？？O hydrogen bonds into dimers, generating rings with graph-set motif R22（8）. Furthermore, a couple of O（7）–H（10）？？？O（3） hydrogen bonds were formed by O atom of P=O and H atom from hydroxyl in the solvent ethanol. Thermal property of the compound was also studied by means of thermogravimetry （TGA）. The thermal analysis and preliminary fireproofing test show that the title compound has good flame retardance.
文摘A novel polyester containing glycolic acid(GA)and 2 hydro 2 oxo 1,3,2 dioxaphosphorinane(TMP)was prepared by ring opening polymerization.The composition and the structure of the titled polymer were investigated by 1H NMR, 13 C NMR,FT IR,EA,and VPO.The influence of time on total conversion and molecular weight was also studied.
文摘The stereoselective synthesis of 2-chloro-4-substituted-phenyl-5,5-dimethyl-1,3,2-dioxaphosphorinan-2-(thi)ones is described. Only single trans-isomers were obtained when 1-substituted-phenyl-2,2-dimethyl-1,3-propanediols (1) reacted with POCl3. But the stereoselectivity of cyclization reaction between (1) and PSCl3 depended greatly upon the reaction condition. The configurational assignments and the ratio of cis-/trans- diastereoisomers of the products were performed on the basis of (HNMR)-H-1, (PNMR)-P-31 and IR spectra and confirmed by X-ray diffraction analyses.
文摘In order to construct the zwitterionic structure of phosphorylcholine onto the surface of biomaterials, five novel phospholanes containing hydroxyl group were synthesized from the corresponding diol and 2-chloro-2-oxo-1,3,2-dioxaphospholane in the presence of THF. Then, five novel phosphorylcholines containing hydroxyl group were prepared by the corresponding phospholane and anhydrous trimethylamine in the presence of acetonitrile. Their structures were characterized by FTIR, 1H NMR and elemental analysis.
