1079-66-9Relevant articles and documents
Facial conversion of secondary phosphine oxides R1R2P(O)H to chlorophosphines R1R2PCl by acetyl chloride
Zhang, Jian-Qiu,Yang, Shangdong,Han, Li-Biao
, (2020)
A practically useful protocol for the reductive transformation of secondary phosphine oxides R1R2P(O)H to chlorophosphines R1R2PCl using acetyl chloride was disclosed. Various secondary phosphine oxides could be readily reduced to the corresponding chlorophosphines in high yields under mild conditions.
Radical-initiated P,P-metathesis reactions of diphosphanes: Evidence from experimental and computational studies
Branfoot, Callum,Young, Tom A.,Wass, Duncan F.,Pringle, Paul G.
, p. 7094 - 7104 (2021)
By combining the diphosphanes Ar2P-PAr2, where Ar = C6H5, 4-C6H4Me, 4-C6H4OMe, 3,5-C6H3(CF3)2, it has been shown that P,P-metathesis generally occurs rapidly under ambient conditions. DFT calculations have shown that the stability of unsymmetrical diphosphanes Z2P-PZ′2 is a function of the difference between the Z and Z′ substituents in terms of size and electronegativity. Of the mechanisms that were calculated for the P,P-metathesis, the most likely was considered to be one involving Ar2P radicals. The observations that photolysis increases the rate of the P,P-metatheses and TEMPO inhibits it, are consistent with a radical chain process. The P,P-metathesis reactions that involve (o-Tol)2P-P(o-Tol)2 are anomalously slow and, in the absence of photolysis, were only observed to take place in CHCl3 and CH2Cl2. The role of the chlorinated solvent is ascribed to the formation of Ar2PCl which catalyses the P,P-metathesis. The slow kinetics observed with (o-Tol)2P-P(o-Tol)2 is tentatively attributed to the o-CH3 groups quenching the (o-Tol)2P radicals or inhibiting the metathesis reaction sterically.
Monoacylphosphine oxides with substituents in the phosphonyl moiety as Norrish I photoinitiators: Synthesis, photoinitiattion properties and mechanism
Duan, Haodong,Gao, Jun,Han, Yuxi,Leng, Kangwei,Li, Qianmin,Liu, Dayong,Wang, Zhongwei,Xu, Xiaolei,Yu, Qing
, (2021/09/07)
In order to study the effect of the substituents in the phosphonyl moiety of monoacylphosphine oxide (MAPO) on its stability and initiation performance, (2,4,6-trimethylphenyl)(phenyl)(benzoyl)phosphine oxide (TMBPO), (4-tolyl)(phenyl)(2,4,6-trimethylbenzoyl)phosphine oxide (4-MTPO) and (2,4-xylyl)(phenyl)(2,4,6-trimethylbenzoyl)phosphine oxide (2,4-DMTPO) were designed and prepared. Studies on TMBPO showed that the introduction of methyl groups into the phosphonyl moiety of MAPO significantly enhanced its stability and light absorption abilities. The photopolymerization of trimethylolpropane triacrylate (TMPTA) showed that the initiation efficiency of 4-MTPO and 2,4-DMTPO were higher than that of TPO, regardless of whether it was initiated upon LED at 385 nm or 420 nm. In addition, the migration rates of 4-MTPO and 2,4-DMTPO in cured TMPTA were approximately 1/2 and 1/4 that of TPO, respectively.
Synthetic method of RRPCl
-
Paragraph 0027-0041, (2020/04/06)
The invention provides a synthetic method of RRPCl, and belongs to the field of organic matter synthesis. The synthetic method of RRPCl solves the problems of low reaction yield and the like in the existing RRPCl synthesis, and is characterized in that RRP(O)H is dissolved in an organic solvent and then reacts with acetyl chloride to obtain the RRPCl, and the chemicalreaction formula of the RRPCl is shown as a formula (I), wherein R1 and R2 are aryl and alkyl. The synthetic method has the advantages of the high yield and the like.
Novel method for synthesizing chlorodiphenylphosphine by one-step process
-
Paragraph 0030; 0032-0039, (2019/07/17)
The invention relates to a novel method for synthesizing chlorodiphenylphosphine by a one-step process. The method comprises the following steps: respectively adding phosphorus trichloride, benzene and aluminum trichloride into a three-necked bottle, performing programmed heating to 140-150 DEG C while stirring under the protection of nitrogen, carrying out a heat insulation reaction at the temperature of 140-150 DEG C until no reflux state, and cooling the obtained reaction solution to room temperature; adding an organic solvent to the reaction solution, performing stirring for several hours,dropwise adding a decomplexing agent, stirring the obtained solution for several hours after the drop-by-drop addition of the decomplexing agent is finished, standing the solution to layer the solution, separating out the obtained decomplexing agent layer, carrying out reduced pressure distillation on the obtained organic solvent layer to obtain crude chlorodiphenylphosphine, and distilling the crude chlorodiphenylphosphine under a high vacuum to obtain pure chlorodiphenylphosphine. The method reduces the environmental pollution by recovering the aluminum trichloride, increases the yield of abyproduct, increases the income, and also has the advantages of high yield, low cost and short reaction time.
Synthesis method of diphenylphosphine chloride
-
Paragraph 0030-0047, (2019/10/01)
The invention discloses a synthesis method of diphenylphosphine chloride, belongs to that technical field of chemical synthesis and solves the problem of low yield of the prior diphenylphosphoric chloride product. The synthesis method of diphenylphosphine chloride is characterized by comprising the following steps: under that protection of dry nitrogen, opening and stirring, adding benzene, phosphorus trichloride and catalyst to a reactor, and raising the temperature to 50 DEG C-80 DEG C and performing reflux reaction at 50 DEG C-80 DEG C for 2-3 h; after the reaction in step S01 is completed, raising the temperature to 85-200 DEG C and performing reflux reaction at 85-200 DEG C; at that end of step S02, after the reactor is cooled down, adding benzene into the reactor, adding a decomplexing agent, stirring until the decomplexing agent is dissolved and distilling to remove benzol, and then performing vacuum distillation to obtain the front fraction and the rear fraction. The inventionhas the advantages of high product yield.
Synthesis and characterization of new PNNP-type chiral ligands
Tezcan, Burcu,Güzel, Bilgehan
, p. 315 - 316 (2018/12/11)
Polydentate ligands having both soft and hard centers are very effective ligands for the preparation of transition metal complexes. PNNP-type tetradentate diaminodiphosphine ligands are most preferred ligand types cause of their good efficiency for the asymmetric reactions. In this study, three different iminophosphine derivative PNNP-type chiral ligands were synthesized using (R)-(+)-1,1′-Binaphthyl-2,2′-diamine (R-BINAM) and d?phenylphosph?no benzaldehyde derivatives.
Method for preparing diarylphosphoryl chloride compound
-
Paragraph 0014-0015, (2018/06/15)
The invention discloses a method for preparing a diarylphosphochlorine compound and belongs to the field of organic synthesis. The method is as follows: the diarylphosphochlorine compound is preparedby reaction of triarylphosphine as a starting material with phosphorus trichloride in the presence of zinc trifluoromethanesulfonate as a catalyst and distillation. Compared with the prior art, the method has the advantages of high reaction yield and simple post-treatment, is particularly suitable for preparation of the diarylphosphochlorine compound with a substituent, and is more suitable for industrial production. The obtained diarylphosphochlorine compound can be used as a ligand for synthesizing metal catalysts, and is applied to the fields such as organic photoelectric materials and medicines.
Method for preparing alkyl phosphine hahalide and reactor for method
-
Paragraph 0117; 0118; 0121; 0122; 0125; 0126, (2019/01/06)
The invention relates to a method for preparing compounds as shown in a formula (I) and a formula (II) which are shown in the description and a reactor specially used for implementing the method. In the formula (I) and the formula (II), X represents halogen, and R represents an alkyl group. The method comprises the step of enabling yellow phosphorus to react with the compound as shown in a formula(III) in a reactor under a condition that no catalyst exists. The method is characterized in that a material on the surface, which is in contact with reaction space, in the reactor is nickel-based alloy used as anti-corrosion alloy, or the reactor is totally formed by the nickel-based alloy used as the anti-corrosion alloy along the whole reaction wall thickness direction. According to the methoddisclosed by the invention, the nickel-based alloy used as the anti-corrosion alloy is adopted as the material of the reactor and accessories of the reactor, an improved anti-corrosion effect betterthan that of an existing reactor and accessories thereof can be realized, and the cost is acceptable, so that the method can be realized in an industrial scale.
A twin-sulfur [...]/aryl heterocyclic compound phosphoric acid as the auxiliary ligand iridium complex of (by machine translation)
-
Paragraph 0033; 0034; 0038, (2018/09/21)
The invention relates to a nitrogen heterocyclic main ligand, in order to double-sulfur [...]/aryl heterocyclic phosphate compound as auxiliary ligand new iridium complex. Iridium complex molecular nitrogen heterocyclic and sulfur group contribute to improving the material of the electron mobility and control light-emitting color, so as to balance the cavity with electronic injection and transmission, widen the carrier composite area, promote the device efficiency, reduce efficiency roll-off. The invention the iridium complex synthetic simple, stable chemical property, easy to sublimation purification, device performance, in order to obtain high efficiency of the organic electroluminescent device and its application in the field of lighting and display provides the convenience. (by machine translation)
