16391-07-4Relevant articles and documents
Daugherty et al.
, p. 95,97 (1968)
Isostructural series of nine-coordinate chiral lanthanide complexes based on triazacyclononane
Walton, James W.,Carr, Rachel,Evans, Nicholas H.,Funk, Alexander M.,Kenwright, Alan M.,Parker, David,Yufit, Dmitry S.,Botta, Mauro,De Pinto, Sara,Wong, Ka-Leung
, p. 8042 - 8056 (2012)
Nonadentate ligands based on triazacyclononane incorporating pyridyl-2-phosphinate groups form an isostructural series of complexes with Ln ions in the solid state and in solution. The Ln ion is effectively shielded from the solvent environment. Crystal structures reveal a rigid C 3-symmetric tricapped trigonal-prismatic coordination geometry that is maintained in solution for the methyl and phenylphosphinate series, as shown by multinuclear NMR analysis. Variable-temperature measurements of the field dependence of the water proton relaxivity in gadolinium complexes indicate that these systems exclude solvent from the primary coordination environment and minimize the second sphere of solvation. The electronic relaxation time for the gadolinium methylphosphinate complex has been estimated to be 550 (±150) ps by EPR and NMR methods, compared to values of around 0.30-0.05 ps for the terbium-ytterbium series, deduced by analyzing the field dependence (4.7-16.5 T) of the 31P NMR longitudinal relaxation times. Values are compared with analogous azacarboxylate ligand complexes, supporting a key role for donor atom polarizability in determining the electronic relaxation. Spectral emission behavior in solution of samarium, europium, terbium, and dysprosium complexes is compared, and the resolved RRR-λ and SSS-Δ complexes show strong circularly polarized luminescence. The molecular quadratic hyperpolarizability βHLS has been measured in solution using hyper-Raleigh light-scattering methods, for the whole series of lanthanide complexes of one ligand. The values of βHLS reach a maximum around the center of the series and are not simply dependent on the number of f electrons, suggesting a dominant contribution from the octupolar rather than the dipolar term.
Synthetic method of methyl hypophosphite
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Paragraph 0043-0045; 0046-0048, (2020/10/30)
The invention relates to a method for synthesizing methyl hypophosphite, which is prepared by reacting methyl phosphine dichloride and alcohol serving as raw materials in a continuous flow reactor. The method is simple in technological process, few in side reaction, capable of reducing generation of toxic substances, low in after treatment cost, high in production efficiency, high in yield and purity, good in safety and suitable for industrial production.
Synthesis method of synthetic intermediate methyl phosphite monoester of glufosinate ammonium
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Paragraph 0075; 0076, (2018/09/08)
The invention belongs to the technical field of synthesis of glufosinate ammonium and in particular relates to a synthesis method of a synthetic intermediate methyl phosphite monoester of glufosinateammonium. Aiming at the common problem of an existing methyl phosphite monoester synthesis method that the cost is too high so that the existing methyl phosphite monoester synthesis method is not applicable to large-scale industrial production, the synthesis method provided by the technical scheme comprises the following steps: [1], enabling methylphosphonothioic dichloride to react with a hydroxyl compound under the action of an alkali A, so as to obtain diethyl methylphosphonothionate; [2], dissolving the diethyl methylphosphonothionate into a solvent B to prepare a diethyl methylphosphonothionate solution; carrying out hydrolysis reaction under the action of an alkali B to generate methylphosphonothioic monoester; [3], dissolving the methylphosphonothioic monoester into a solvent C to prepare a methylphosphonothioic monoester solution; carrying out desulfurization reaction on the methylphosphonothioic monoester solution under the action of a catalyst to prepare the methyl phosphitemonoester. The synthesis method provided by the invention is applicable to a glufosinate ammonium synthesis industry.
