Containing phosphorus preparation

Phosphonic acid, H3PO3, often called just phosphorous acid , is prepared by the hydrolysis of phosphorus trichloride a stream of air containing phosphorus trichloride vapour is passed into ice-cold water, and crystals of the solid acid separate ... 

Although most of the macrocycles that contain phosphorus or arsenic which have thus far been prepared, are primarily transition metals binders, two compounds have been prepared which are essentially crown ethers containing phosphorus. Kudrya, Shtepanek and Kirsanovhave prepared two compounds which are essentially polyoxygen macrocycles but which contain one or two methylphosphonic acid esters as part of the ring. These two macrocycles are shown below as 7d and 17 and are both prepared by the reaction of 2,2 [oxybis(ethyleneoxy)] bisphenolate with methylphosphonic dichloride in a mixture of acetonitrile and benzene. The crystalline monomer 16) and dimer 17) were isolated in 17% and 11% yields respectively as indicated in Eq. (6.13). 

B. Electrophilic Reactions.—Transesterification followed by rearrangement is a common route from simple phosphites to more complex phos-phonates. This has now been applied to the preparation of cyclic phos-phonates (85). Both phosphites (86) and phosphoranes (87) containing phosphorus-hydrogen bonds are obtained from the cyclic biphosphite (88) and butanol. ... 

In a study of dental silicate cements, Kent, Fletcher Wilson (1970) used electron probe analysis to study the fully set material. Their method of sample preparation varied slightly from the general one described above, in that they embedded their set cement in epoxy resin, polished the surface to flatness, and then coated it with a 2-nm carbon layer to provide electrical conductivity. They analysed the various areas of the cement for calcium, silicon, aluminium and phosphorus, and found that the cement comprised a matrix containing phosphorus, aluminium and calcium, but not silicon. The aluminosilicate glass was assumed to develop into a gel which was relatively depleted in calcium. 

The most important acid containing phosphorus is orthophosphoric acid, H3P04. This is the acid usually indicated when the name phosphoric acid is used in most contexts. Approximately 30 billion pounds of this acid are produced annually. The commercial form of the acid is usually a solution containing 85% acid. The process used to produce phosphoric acid is related to the intended use of the acid. If the acid is intended for use in foods, it is prepared by burning phosphorus and dissolving the product in water. 

Preparation, Characterisation and Properties of Compounds Containing Phosphorus-Chalcogen Bonds... 

One of the first results on the use of phosphine dendrimers in catalysis was reported by Dubois and co-workers [16]. They prepared dendritic architectures containing phosphorus branching points which can also serve as binding sites for metal salts. These terdentate phosphine-based dendrimers were used to incorporate cationic Pd centers in the presence of PPh3. Such cationic metalloden-dritic compounds were successfully applied as catalysts for the electrochemical reduction of C02 to CO (e.g. 9, Scheme 9) with reaction rates and selectivities comparable to those found for analogous monomeric palladium-phosphine model complexes suggesting that this catalysis did not involve cooperative effects of the different metal sites. 

Preparation of Phosphorus Containing Terpolymers. Prepared by substitution of a portion of the acid chloride mixture by a calculated amount of phenyl phosphonic dichloride. The compositions of these polymers are summarized in Table 1. 

Harris, R. K., Woplin, J. R, Murray, M., Schmutzler, R. Preparation and nuclear magnetic resonance spectra of symmetrical spin systems containing phosphorus bis(fluorophosphinothioyl) sulfides. J. Chem. Soc. Dalton 1972, 1590. 

Sulphuric, ae.id containing phosphorus peulnxide. Approximately 10, 15, or 20 per cent of I>. are the usual strengths. The. preparation is employed in Kjeldnhl s nitrogen determination. 

Fuming sulphuric acid containing phosphorus pentoxide the usual grades contain approximately 5, 10, 15, 20, or 25 per cent of P2Ot. The preparation is used in Kjeldahl s nitrogen determination. 

Compounds containing phosphorus can be both valuable synthetic intermediates and target compounds of solid-phase synthesis. Important synthetic intermediates include phosphonium salts and phosphorus ylides, which are key intermediates in carbonyl olefinations. Their preparation is discussed in Section 5.2.2.1. The preparation of oligonucleotides, these being the most important phosphorus-containing target molecules in solid-phase synthesis, is considered in Section 16.2. In this chapter, the preparation of phosphines, phosphonic acid derivatives, and phosphinic acid derivatives is discussed. 

The early workers on phosphorus prepared that element from urine which normally contains ammonium and sodium phosphates. Thus, R. Boyle1 evaporated the urine to a syrupy consistency, and distilled the product either alone or admixed with sand or charcoal. The carbon produced by the decomposition of the organic matter in the urine, or added to it in the form of charcoal, decomposes the ammonium phosphate, without affecting the sodium phosphate. A. S. Marggraf mixed the cone, urine with lead chloride and charcoal powder, and heated the mass until it became pulverulent. The ammonium and sodium phosphates were converted into lead phosphate, and on distillation, the carbon liberated the phosphorus from the lead phosphate. G. A. Giobert mixed the unevaporated urine with lead nitrate or acetate washed the precipitated mixture of lead phosphate and sulphate mixed the precipitate with charcoal and distilled the dried product. 

Ionene, a commercial fragrance, has been prepared traditionally by treatment of a- and /3-iononcs with hydriodic acid containing phosphorus or by distillative heating in the presence of 0.5% iodine. In an unoptimized demonstration, cyclization occurred more cleanly and simply by MBR with /3-ionone in water at 250 °C (Scheme 19) [83]. Work-up also was facilitated, as the need for removal of catalyst or the formation and separation of bi-products was avoided. At elevated temperature, the addition of water to olefins can occur readily, without adding catalyst. (S)-(+)-carvone in water for 10 min at 180 °C afforded optically pure 8-hydroxy-p-6-mcnlhcn-2-one as an intermediate toward carvacrol [84], Addition of water across the 8,9-double bond of carvone occurred regioselectively, by Markovnikov addition. Carvacrol itself was obtained almost quantitatively from carvone at 250 °C after 10 min (Scheme 19) [84]. 

Magnesium phosphide was first obtained from the metal and organic substances containing phosphorus,5 but is best prepared by heating the metal in phosphorus vapour or with red phosphorus in an atmosphere of hydrogen.6,7... 

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