66295-44-1Relevant academic research and scientific papers
Preparation method of dialkyl methylphosphonite
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Paragraph 0055-0063, (2018/02/04)
The invention relates to a preparation method of dialkyl methylphosphonite. tertiary amine with pKa greater than 10 is adopted as the acid binding agent, methyl phosphonic dichloride and alcohol react in a solvent, and the mole ratio of the methyl phosphonic dichloride, alcohol and tertiary amine is 1:2.0-2.4:2.0-2.4, the produced tertiary amine hydrochloride is neutralized with a caustic soda aqueous solution, and the solvent and tertiary amine obtained by evaporation is recycled and reused. The alkyl of the dialkyl methylphosphonite is straight chain and side chain alkane or alkene of aliphatic C1-C4, the alcohol refers to methanol, ethanol, propanol, isopropanol, allyl alcohol, n-butanol, isobutanol and the like, the tertiary amine refers to tertiary fatty amine, and also refers to fatty group and aromatic mixed tertiary amine, at the same time, the pKa of the tertiary amine is required to be greater than 10, and the tertiary amine can include triethylamine, tripropylamine and tributylamine.
POLYOXYDES DE POLYPHOSPHINES BICYCLIQUES ALKYLES SUR LE PHOSPHORE
Toulhoat, C.,Vidal, M.,Vincens, M.
, p. 119 - 132 (2007/10/02)
In the preparation of γ and β- tracers for use in biomedical measurement, we have studied the reaction between two alkylated dioxophosphides and o-xylene-α,α'-dichloride 5.The dioxophosphides are prepared by reaction of diisopropylethylenediphosphinate 1 or diisopropyltrimethylenediphosphinate 2 with sodium bis(methoxyethoxy)aluminohydride (vitride).The cycloaddition reactions give predominantly the 1/1 cyclocondensation compounds 6 and 9; 2/2 and 3/3 cyclocondensation products 7, 8, 10 are also obtained but in significantly lower yield.The yield of the 1/1 product can be optimized when the reaction is monitored by 31P NMR.The 1/1 products are mixtures of diastereoisomers which have been identified.The cyclic diphosphines 11 are obtained by reduction of the corresponding cyclic phosphine dioxides using LiAlH-CeCl3. Key words: Diphosphine dioxide; alkylated phosphines; cyclocondensations; P=O intracyclic reduction.
Polyoxides de polyphosphines macrocycliques P-alkyles
Toulhoat, C.,Vincens, M.,Vidal, M.
, p. 647 - 654 (2007/10/02)
With the aim of obtaining complexes of γ-emitters and paramagnetic ions for use as imaging reagents and contrast agents, the synthesis of ligands was performed by cyclocondensation between dioxophosphids, α,ω-dihalogenoalkanes, and alkenes.These reactions lead to new cyclic P-alkylated polyphosphine polyoxides with saturated and unsaturated bridges.The 1:1 cyclocondensation products are obtained predominantly over the 2:2 and 3:3 cyclocondensation products.The formation of tetraphosphorated cycles becomes significant when it is allowed by the dihalide configuration.The origin of these orientations is discussed and a mechanism is als o presented for these reactions.Key words: cyclocondensation; cyclic polyphosphine polyoxide; dioxodiphosphid; α,ω-dihalide; P-alkylated phosphorus macrocycle
LES PHOSPHORANES MONOCYCLIQUES A LIAISON PH DANS LES REACTIONS DE REDISTRIBUTION DE LIGANDS DES COMPOSES DU PHOSPHORE TRICOORDONNE
Tangour, B.,Malavaud, C.,Boisdon, M. T.,Barrans, J.
, p. 189 - 196 (2007/10/02)
The oxidative addition of alcohols and amines with 2-alkyl, 2-aryl, 1,3,2-dioxa, oxaza or diazaphospholanes, leads to a ring opening reaction and ligands exchange around the phosphorus atom by alcoholysis or aminolysis of P-O or P-N bonds.In nearly all cases, monocyclic phosphoranes with P-H bond have been detected in an intermediate step during the exchange of one tricoordinate form to another one.At last we have discussed the phorpholanyl ring stability. - Key words: 1,3,2-Dioxaphospholanes; 1,3,2-oxaza-phospholanes; 1,3,2-diazaphospholanes; Monocyclic phosphoranes with P-M bonds; phosphoranyl ring stability.
