Showing papers on "Dichlorophenylphosphine published in 2013"

A convenient synthesis and spatial structure of 2-aryl-2-oxo-2-phenylbenzo[e]-1,4,2-oxazaphosphinanes

Abstract: Phosphorylation of 2-arylideneaminophenol with dichlorophenylphosphine in the presence of triethylamine and subsequent treatment with water led to stereoisomeric derivatives of 3-aryl-2-oxo-2-phenylbenzo[e]-1,4,2-oxazaphosphinanes, which were separated by column chromatography to the individual diastereomers. The structure of stereoisomers was established by NMR spectroscopy and X-ray crystallography.

Phenyldipropylphosphinate compound and preparation method thereof

Abstract: The invention relates to a phenyldipropylphosphinate compound and a preparation method thereof The structure of the compound is shown in the specification The preparation method comprises the following steps of: controlling the molar ratio of dichlorophenylphosphine to sodium n-propoxide; dropwise adding the dichlorophenylphosphine into a solution of an organic solvent of sodium n-propoxide with certain concentration at 10 DEG C; after dropwise adding, controlling the temperature at 15-20 DEG C, and stirring for reaction for 1-2 hours; heating to 40-50 DEG C, and preserving heat for reaction for 2-3 hours; filtering to remove NaCl; distilling out the organic solvent; and performing reduced-pressure distillation and collecting the fraction at 118-120 DEG C under a pressure of 133KPa to obtain phenyldipropylphosphinate The product provided by the invention is a halogen-free organic phosphine flame retardant, has high flame retardance, is suitable to be used as a flame retardant of materials such as polyurethane, epoxy resin, unsaturated resin and the like, and also serves as an intermediate for synthesis of organic phosphine According to the phenyldipropylphosphinate compound and preparation method thereof provided by the invention, the technology is simple, the equipment investment is small, and the industrial production is facilitated

AlCl3·XNaCl Complex Compound as Catalyst Synthesis Dichlorophenylphosphine

Abstract: Dichlorophenylphosphine(DCPP) was prepared by the catalyst of AlCl3·XNaCl complex using C6H6, PCl3 as raw materials. The influences of the catalyst amount, raw material ratio and the choice of extractant on the production rate were studied, as well as the recycling of the catalyst. Fourier transform infrared spectroscopy was employed to characterize the products. The results show that the products by experiments were dichlorophenylphosphine(DCPP). All above have some reference value for the industrial production.

Phenyldipropylphosphinate compound and preparation method thereof

Abstract: The invention relates to a phenyldipropylphosphinate compound and a preparation method thereof. The structure of the compound is shown in the specification. The preparation method comprises the following steps of: controlling the molar ratio of dichlorophenylphosphine to sodium n-propoxide; dropwise adding the dichlorophenylphosphine into a solution of an organic solvent of sodium n-propoxide with certain concentration at 10 DEG C; after dropwise adding, controlling the temperature at 15-20 DEG C, and stirring for reaction for 1-2 hours; heating to 40-50 DEG C, and preserving heat for reaction for 2-3 hours; filtering to remove NaCl; distilling out the organic solvent; and performing reduced-pressure distillation and collecting the fraction at 118-120 DEG C under a pressure of 1.33KPa to obtain phenyldipropylphosphinate. The product provided by the invention is a halogen-free organic phosphine flame retardant, has high flame retardance, is suitable to be used as a flame retardant of materials such as polyurethane, epoxy resin, unsaturated resin and the like, and also serves as an intermediate for synthesis of organic phosphine. According to the phenyldipropylphosphinate compound and preparation method thereof provided by the invention, the technology is simple, the equipment investment is small, and the industrial production is facilitated.

Synthesis method for dichlorophenylphosphine oxide

Abstract: The invention provides a synthesis method for dichlorophenylphosphine oxide, relating to a synthesis method for a catalyst for chemical industry. The synthesis method comprises the following steps of taking benzene and phosphorus trichloride as raw materials and simultaneously adding sodium chloride and alchlor as the catalyst, reacting so as to produce mixed liquor of the dichlorophenylphosphine oxide, benzene and the phosphorus trichloride and solid residue, processing the solid residue with extracting agent and mixing with the mixed liquor, thus obtaining the pure dichlorophenylphosphine oxide through distillation under normal pressure and reduced pressure. The catalyst AlCl3*XNaCl complex can be recycled. Compared with traditional method, the synthesis method has the characteristics that the operation steps are simple, the production time is short, decomplexing agent is added no more in the steps, the synthesis method is easy to operate and control, the production cost is low, and the production steps are environment-friendly, and the like.

Synthesis method for dichlorophenylphosphine oxide

Abstract: The invention provides a synthesis method for dichlorophenylphosphine oxide, relating to a synthesis method for a catalyst for chemical industry. The synthesis method comprises the following steps of taking benzene and phosphorus trichloride as raw materials and simultaneously adding sodium chloride and alchlor as the catalyst, reacting so as to produce mixed liquor of the dichlorophenylphosphine oxide, benzene and the phosphorus trichloride and solid residue, processing the solid residue with extracting agent and mixing with the mixed liquor, thus obtaining the pure dichlorophenylphosphine oxide through distillation under normal pressure and reduced pressure. The catalyst AlCl3*XNaCl complex can be recycled. Compared with traditional method, the synthesis method has the characteristics that the operation steps are simple, the production time is short, decomplexing agent is added no more in the steps, the synthesis method is easy to operate and control, the production cost is low, and the production steps are environment-friendly, and the like.

Preparation method of aluminum phenylphosphinate

Abstract: The invention discloses a preparation method of aluminum phenylphosphinate. The preparation method comprises the following steps: a. preparing 0.1-1mol/L aluminum nitrate or aluminum sulfate solution; b. slowly dropping the aluminum nitrate or aluminum sulfate solution in dichlorophenylphosphine at 0-40 DEG.C; c. after dropping, heating and adjusting the pH value of the solution, reacting for 1-3 hours at 40-100 DEG.C to generate a target product aluminum phenylphosphinate. The method disclosed by the invention is used for preparing aluminum phenylphosphinate by adopting aluminum nitrate or aluminum sulfate solution and dichlorophenylphosphine to directly react under acidic condition in one-step method, the yield of the target product is 87-96%; the obtained aluminum phenylphosphinate is white powder, the color treatment is unnecessary, and the purity is high; the existing process rout is simplified, the reaction time is short, the environment-friendly is realized, the cost is low, and the method is more suitable for the industrial production.

tert‐Butyl(phenyl)phosphinothioic acid

Abstract: Racemate [6002-45-5] InChI = 1S/C10H15OPS/c1-10(2,3)12(11,13)9-7-5-4-6-8-9/h4-8H,1-3H3,(H,11,13) InChIKey = ACQNBIJCKLUKMY-UHFFFAOYSA-N (S)-Enantiomer [55705-77-6] InChI = 1S/C10H15OPS/c1-10(2,3)12(11,13)9-7-5-4-6-8-9/h4-8H,1-3H3,(H,11,13)/t12-/m1/s1 InChIKey = ACQNBIJCKLUKMY-GFCCVEGCSA-N (R)-Enantiomer [54100-47-9] C10H15OPS (MW 214.26) InChI = 1S/C10H15OPS/c1-10(2,3)12(11,13)9-7-5-4-6-8-9/h4-8H,1-3H3,(H,11,13)/t12-/m0/s1 InChIKey = ACQNBIJCKLUKMY-LBPRGKRZSA-N (precursor to various optically pure phosphines, resolving agent, and chiral solvating agent) Physical Data: mp 95–96 °C. Solubility: soluble in dichloromethane, ethanol, and most organic solvents. Form Supplied in: crystalline solid. Preparative Method: racemic tert-butyl(phenyl)phosphinothioic acid is synthesized by reacting dichlorophenylphosphine with tert-butylmagnesium chloride followed by refluxing with molecular sulfur in toluene. Resolution involves treatment with (S)-(−)-α-methylbenzylamine in ether followed by collection of the crystalline, ether-insoluble (R)-(+)-acid-(S)-(−)-amine salt. If the NMR spectrum shows contamination from the diastereomeric salt, the salt is dissolved in chloroform and induced to recrystallize by addition of ether. The crude (−)-acid was recovered from the ether-soluble (S)-(−)-acid-(S)-(−)-amine salt (eq 1).1 (1) Handling, Storage, and Precautions: storage in a cool, dry place is recommended.