2428-06-0Relevant articles and documents
Synthesis and Solubility of 5,5-Dimethyl-2-(phenyl(phenylamino)methyl)-1,3,2-dioxaphosphinane 2-oxide in Selected Solvents between 278.15 K and 347.15 K
Ma, Xiao,Zhao, Qianqiong,Liu, Qianwen,Xing, Yalin,Fan, Ruilan,Tian, Rongkai
, p. 4196 - 4204 (2017)
A flame retardant with enhanced phosphorus-nitrogen content, 5,5-dimethyl-2-(phenyl(phenylamino)methyl)-1,3,2-dioxaphosphinane 2-oxide (DPPO), was synthesized by the reaction of 5,5-dimethyl-1,3,2-dioxaphosphinane 2-oxide (DDPO) with N-benzylideneaniline. The structure of DPPO was characterized by nuclear magnetic resonance (1H NMR and 31P NMR) and Fourier transform infrared (FT-IR) spectroscopy. The thermal stability of DPPO was characterized by thermogravimetric analysis (TGA). The solubilities of DPPO were measured in different solvents including ethyl acetate, methanol, chloroform, acetonitrile, acetone, 1,2-dichloroethane, 1,4-dioxane, dichloromethane, tetrachloromethane, benzene, tetrahydrofuran, and isopropanol at temperature ranging from 278.15 to 347.15 K by the gravimetrical method. The mole fraction solubilities of DPPO in the above-mentioned organic solvents were correlated as the Apelblat equation, and the calculated values with equations shows good consistency with the experimental values. The root-mean-square deviation was less than 0.1%, and the average relative error was less than 0.04 in all of the experiments.
New synthetic route and characterisation of phosphorus and arsenic heterocyclic compounds
Matos, Robson M.,Gomes De Lima, Luiz Carlos,De Souza, Edward,Barcelos De Souza, Ana Lucia Americano,Gomes De Lima, Miriam Bernardes,Soares Raslan, Delio
, p. 2859 - 2870 (2002)
Herein we report synthetic routes for the preparation of 2-chloro-1,3,2-dioxarsenane 1, O,O′-bis(5,5-dimethyl-1,3,2-dioxarsenane)-2,2-dimethyl-1,3-propanediol 3, 2-chloro-1,3,2-dioxaphosphorinane 4, and 2-fluoro-1,3,2-dioxaphosphorinane 5. The new synthetic routes described here have the advantage to be simple, very clean and to lead to the desired compounds in very good yields. Compound 2-fluoro-1,3,2-dioxarsenane 2 also was prepared in good yield and is described here for the first time. Compounds 1-5 were fully characterized on the basis of NMR spectroscopic studies. Semi-empirical structural studies have been carried out and the results show that 1 and 2 exist as a mixture of two conformers, whereas only one conformer for 4 and 5 have been found. Variable temperature 1H NMR studies reveal a fluxional behaviour for 1 and a mechanism for the inter-conversion between its two conformers is proposed.
Phosphate-phosphonate preparation method
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Paragraph 0086; 0087; 0088; 0089; 0090-0093, (2019/01/08)
The invention relates to a phosphate-phosphonate preparation method, which comprises the following steps: performing condensation and dehydration reaction on neopentyl phosphite and alcohol phosphonate in the presence of an esterification catalyst, then adding ozone for oxidation, and distilling a solvent under reduced pressure to obtain the phosphate-phosphonate, the neopentyl phosphite being generated by hydrolyzing neopentyl phosphorochloridite. According to the method, use of a triethylamine acid binding agent is avoided, so that problems about recovery and pollution of a large amount of triethylamine hydrochloride are reduced; the mild ozone is adopted as an oxidizer, so that simplicity and convenience are ensured, explosion dangers of hydrogen peroxide are avoided, the reaction condition is mild and easy to control, and the ozone subjected to aftertreatment can be conveniently and rapidly treated directly by illumination; time for oxidation reaction is greatly shortened, the reaction temperature is low, and the purity and the yield of an obtained product are high, and are greatly improved compared with those achieved by a conventional process.
Allenylphosphonates/allenylphosphine oxides as intermediates/precursors for intramolecular cyclization leading to phosphorus-based indenes, indenones, benzofurans, and isochromenes
Sajna,Kumara Swamy
body text, p. 5345 - 5356 (2012/08/27)
Utilizing internally available functional groups, a simple protocol for the efficient synthesis of phosphorus-based indenes, indenones, benzofurans, and isochromenes via intramolecular cyclization of allene intermediates/precursors is generated; the latter intermediates/precursors are conveniently obtained through aldehyde-, alkylidene-, and hydroxyl-functionalized propargyl alcohols and PIII-Cl precursors. The structures of key products have been unequivocally confirmed by X-ray crystallography.
