2466-73-1Relevant academic research and scientific papers
Method for preparing monoalkyl hypophosphite
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Paragraph 0035; 0036; 0037, (2017/09/18)
The invention relates to a method for preparing monoalkyl hypophosphite. The method comprises the steps of oxidizing monoalkyl hydrogen phosphide halate solution by virtue of hydrogen peroxide, wherein the molar ratio of the monoalkyl hydrogen phosphide halate solution to hydrogen peroxide is 1 to 2 or 1 to 2.1, and the reaction temperature is between (-50)-(20) DEG C. The molecular formula of monoalkyl hypophosphite is RP(H)OOH, wherein R is C1-C10 straight-chain, branched-chain alkyl groups. The method for preparing monoalkyl hypophosphite has the beneficial effects that the reaction yield is more than 80%, and water and halogen hydride can be easily evaporated at a reduced pressure after the reaction is finished and can be recycled by virtue of a sodium hydroxide solution and are not the main content of the invention, so that the method described by the invention is safe, environment-friendly and economic.
Surface properties of butanol phosphate esters in alkali solutions
Du, Zong-Liang,Zhou, Dong-Liang,Chen, Yong,Chen, Min,Zhu, Pu-Xin
experimental part, p. 201 - 206 (2011/10/11)
Phosphate esters of two butanol isomers were synthesized by esterification of n-butanol and isobutanol with phosphorus pentoxide. The surface activity and penetrability of the esters were analyzed by way of surface chemistry and canvas disc wetting tests in different alkaline solutions. The surface tension of the butanol phosphate esters and their sodium salts was found to decrease with increasing alkaline concentration up to 250 g/L NaOH. Furthermore, the products exhibited a good surface activity with proper penetrability even in highly alkaline solutions. The stable surface activity of the esters in concentrated alkali lye interpreted by the adsorption of the molecule from solution owing to the common ion effect. AOCS 2009.
Determination of phosphoric acid mono- and diesters in municipal wastewater by solid-phase extraction and ion-pair liquid chromatography-tandem mass spectrometry
Quintana, Jose Benito,Rodil, Rosario,Reemtsma, Thorsten
, p. 1644 - 1650 (2008/02/05)
The first analytical method for the determination of 13 phosphoric acid mono- and diesters from aqueous samples is presented. The method consists of solid-phase extraction (SPE) and ion-pair liquid chromatographic separation with tri-n-butylamine coupled to electrospray ionization tandem mass spectrometry in the negative ion mode. Due to a lack of pure standards, only 3 of the 13 esters could be quantified. SPE recoveries ranged from 71 to 112% for di-n-butyl phosphate, diphenyl phosphate, and di-(2-ethylhexyl) phosphate (DEHP) with limits of quantification from 7 to 14 ng/L for 100-mL samples. At analyte concentrations ≥1 μg/L, aqueous samples can be analyzed by direct injection without extraction. In municipal wastewater, six diesters and one monoester were unambiguously identified by comparison with synthesized reference material. DEHP showed highest concentrations of 60 and 5 μg/L in raw and treated wastewater, respectively. The detection of monoethylhexyl phosphate was confirmed by LC-Q-TOF-MS analysis, and it was found at a concentration level comparable to DEHP. Laboratory degradation tests show that phosphoric acid diesters can be formed as intermediates in the microbial degradation of trialkyl phosphates that are being used as flame retardants and plasticizers.
Oxidative cleavage of o-hydroxyphenyl phosphate by iodobenzene diacetate
Wu, Pei-Lin,Chen, Jhy-Hong,Huang, Ded-Shih
, p. 967 - 970 (2007/10/03)
The protecting o-hydroxyphenyl group in the synthesis of mono- or dialkyl phosphates (6 or 8) could be removed by oxidative cleavage of mono- or dialkyl o-hydroxyphenyl phosphates (3 or 7) using iodobenzene diacetate.
CONVENIENT SYNTHETIC ROUTE TO MONO- OR DIAKLYL PHOSPHATE FROM INORGANIC PHOSPHORUS ACIDS
Okamoto, Yoshiki,Kusano, Tetuya,Takamuku, Setsuo
, p. 195 - 200 (2007/10/02)
Mono- or dialkyl phosphate was synthesized in a favorable yield by oxidation of phosphonic or phosphinic acid in alcohol with oxygen at the presence of a catalytic amount of copper(II)chloride.The reaction may proceed via the formation of corresponding phosphorochloridate or phosphorochloridite.
The Selective Dealkylation of Mixed Esters of Phosphoric Acid and Phenylphosphonic Acid Using Cation Exchange Resin
Nitta, Yoshihiro,Arakawa, Yasushi
, p. 3121 - 3129 (2007/10/02)
Cation exchange resin (SO3H) is a highly selective dealkylation reagent for mixed esters of phosphorus oxyacids bearing primary and secondary alkyl groups.The desired products which were produced by dealkylation of the secondary alkyl group were obtained in high yields under anhydrous and mild conditions.Keywords - dealkylation; cation exchange resin; carbonium ion; phosphorus oxyacid ester; trialkyl phosphate; dialkyl phenylphosphonate; p-toluenesulfonic acid
MECHANISMUS DER ALKYLIERUNG VON PHOSPHORSAEUREDIETHYLESTER MIT TRIALKYLPHOSPHITEN
Markowska, Anna,Olejnik, Jadwiga
, p. 245 - 254 (2007/10/02)
Alkylation of diethyl phosphoric acid with various trialkyl phosphites was studied by NMR-spectroscopy and conductometry.Ethylation and neopentylation was confirmed to involve corresponding phosphonium salts as intermediates.Intermediacy of mixed PIII-PIV-anhydride in 2-chloroethylation was observed.Mechanistic generalisation of the obtained experimental data has been proposed.
