- Distribution and elimination of 14C-ethion insecticide in chamomile flowers and oil
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The residual fate of 14C-ethion labeled at the ethyl group in chamomile flowers and oil was studied. 14C-ethion and some of its degradation products have been prepared for the present investigation. 14C-residues in its flowers and oil were determined at different time intervals. Chromatographic analysis of chamomile oil extracts revealed the presence of the parent compound together with four metabolites, which were identified as ethion monooxon, ethion dioxon, O,O-diethyl phosphorothioate, and O-ethyl phosphorothioate. Effect of drying on ethion residues in chamomile flowers was investigated. Ethion residues were decreased by sun drying of chamomile flowers. The percentage of removal was 18%-47%. Effect of using low cost adsorbents for removal of ethion residues from chamomile oil was investigated. The removal percentage due to adsorption was 100% for CaO and saw dust adsorbers and for watermelon peels, bagass, and rice bran adsorbers were 36%, 41%, and 90%, respectively. Our results proved that the addition of CaO saw dust and rice bran reduced the pesticide residues, so we recommend the addition of these adsorbents during the extraction process to reduce the risk of pesticide residues on chamomile oil. Copyright Taylor & Francis Group, LLC.
- Abdel-Gawad,Abdelhameed,Elmesalamy,Hegazi
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Read Online
- Diazinon hapten and artificial antigen, preparation method and application thereof
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The invention relates to a diazinon hapten and an artificial antigen, a preparation method and application thereof. The preparation method comprises the following steps of: taking thiophosphoryl chloride as an initiator, reacting thiophosphoryl chloride with ethanol in an alkaline environment, and then carrying out reactione with (2-isopropyl-6-oxo-1, 6-dihydro-4-pyrimidinyl)acetic acid to obtaina compound containing a carboxyl group, namely a diazinon hapten; and coupling the hapten with a carrier protein to obtain the artificial antigen. Animals immunized by using the artificial antigen cangenerate specific antibodies aiming at diazinon, and the specific antibodies can be used for establishing an enzyme-linked immunosorbent assay method of diazinon and a colloidal gold test strip rapiddetection method, so that residues of diazinon in vegetables and fruits can be rapidly detected.
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Paragraph 0025; 0026
(2020/10/04)
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- Green synthesis technology of O,O-diethyl thiophosphoryl chloride
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The invention provides a green synthesis technology of O,O-diethyl thiophosphoryl chloride and relates to the field of chemical synthesis. The green synthesis technology comprises the following steps:taking O,O-diethyl dithiophosphate to react with chlorine gas at low temperature, so as to obtain a crude product of the O,O-diethyl thiophosphoryl chloride; then transferring the crude product to react at high temperature; enabling the residual O,O-diethyl dithiophosphate to further completely react with the chlorine gas. Meanwhile, in a high-temperature reaction process, a polymeric compound isprevented from being generated when a compound catalyst is used and sulfur monochloride impurities are completely removed through reaction, so that a byproduct sulfur has a crystalline state and a product more easily separated and purified. Moreover, HCl and sulfur-containing odorous gas are pumped away through applying negative pressure and the tail gas is absorbed to prevent air pollution. In awhole reaction process, technological water does not need to be added, so that wastewater is not generated and the treatment cost of sulfur-containing and phosphorus-containing wastewater is reduced.The technology has the advantages of simplicity in operation, easiness for obtaining raw materials, moderate reaction conditions, small pollution and environment friendliness.
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Paragraph 0029; 0032-0036; 0039-0043; 0046-0050; 0053-0056
(2019/03/06)
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- Synthesis method of O, O-dialkyl thiphosphoryl chloride
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The invention discloses a synthesis method of O, O-diakyl thiphosphoryl chloride. In a reaction system where O, O-dialkyl S-hydro-phophorodithioate and chlorine are subjected to a chlorination reaction to prepare O, O-dialkyl thiphosphoryl chloride, an excess chlorine is introduced to make sulphur generated in the reaction be converted into disulfur dichloride, and disulfur dichloride is convertedinto sulfur dichloride afterwards; and by controlling the reaction temperature and arranging the reaction system to be in the negative pressure state, sulfur dichloride is moved out of the reaction system in the reaction process through distillation and condensing. The synthesis method substantially achieves the atomic economy based on a green chemistry concept; the overall cost of raw materialsis far lower than that in a traditional method, the amount of the three wastes is less, and the three wastes are easy to dispose; a traditional solid-liquid separation step is cancelled, automated production is facilitated, and meanwhile, improvement of the safety and environment production level of the device is facilitated; and O, O-dialkyl thiphosphoryl chloride is not in contact with water, disintegration of the product is avoided, the yield rate is as high as 93%, and the product content can reach 99%.
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Paragraph 0042; 0043; 0048-0051
(2018/08/28)
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- Organophosphorus hapten, wide-spectrum polyspecific antigen, antibody and preparation method and application of hapten, antigen and antibody
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The invention discloses an organophosphorus hapten, a wide-spectrum polyspecific antigen, an antibody and a preparation method and application of the hapten, the antigen and the antibody. The technical defect of an existing organophosphorus pesticide residue immunity analysis method is overcome, the organophosphorus wide-spectrum polyspecific immunity analysis concept is provided, and for organophosphorus pesticides, the method is good in accuracy and sensitivity, can be used for detecting organophosphorus in agricultural products and food samples, realizes universal wide-spectrum polyspecific detection and is quite convenient and rapid to implement in actual use. The wide-spectrum polyspecific antigen has the structure shown in the formula (III) (the formula is shown in the description).
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Paragraph 0058
(2017/12/06)
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- O,O-diethyl chlorothiophosphate and preparation method thereof
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The invention discloses an O,O-diethyl chlorothiophosphate and a preparation method thereof, belonging to the technical field of insecticides. The preparation method comprises the following steps: mixing and stirring phosphorus pentasulfide and O,O-diethyl dithiophosphate, dripping a mixture of absolute ethyl alcohol and a catalyst A, preserving heat for 10 to 50min, and then filtering to obtain O,O-diethyl dithiophosphate, wherein the catalyst A is prepared from at least one of triethylamine, pyridine, ethylenediamine and carbonate; stirring the O,O-diethyl dithiophosphate at 30 to 50 DEG C, and introducing chlorine to obtain an intermediate product; heating the intermediate product to 80 to 100 DEG C, adding water, performing stirring reaction for 1 to 3h, then performing suction filtration, and enabling filtrate to stand, thus layering to obtain an oil phase and a water phase; dehydrating the oil phase, then evaporating, and collecting a fraction. The preparation method is capable of avoiding side reaction and reducing a reaction residue amount. In addition, the invention provides the O,O-diethyl chlorothiophosphate prepared by using the method.
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Paragraph 0033-0046; 0047-0053; 0054-0060; 0061-0067
(2018/01/04)
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- Production method for O,O-dialkyl thiophosphoryl chloride
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The invention relates to a production method for O,O-dialkyl thiophosphoryl chloride, and belongs to the field of manufacturing of O,O-dialkyl thiophosphoryl chloride through a chemical method. Raw materials comprise dialkyl phosphite, sulfur or sulfide, chlorine or a chlorinating agent and the like. The production method comprises the steps: carrying out a reaction of dialkyl phosphite and sulfur or sulfide in a synthesis kettle for 2 hours, then chloridizing by chlorine or the chlorinating agent to obtain an O,O-dialkyl thiophosphoryl chloride crude product, and then washing with water to obtain the product O,O-dialkyl thiophosphoryl chloride. The total yield can reach 98%-99%, the content of O,O-dialkyl thiophosphoryl chloride can reach more than or equal to 99.5%, the product quality is good, and the purity of the product can reach 99-99.9%; and the production method has the advantages of simple production process, safe production, low energy consumption, and no pollution. The problems in the prior art that a large amount of alcohol is needed to be recycled, consumption of steam is high and energy consumption is high are solved; and the problems that all the process routes need freezing, a large amount of freezing energy and circulating water is needed and the electric energy consumption is high are solved.
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Paragraph 0023; 0024; 0026
(2017/08/27)
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- Synthetic method of methyl phosphite and glufosinate-ammonium
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The invention discloses a synthetic method of methyl phosphite and glufosinate-ammonium. The method comprises the steps: with phosphorus pentasulfide as a starting material, then carrying out vulcanization reaction, chlorination reaction, water washing and distillation purification, then carrying out catalytic hydrogenation to obtain chloride phosphite (III), and next carrying out Grignard reaction to obtain methyl phosphite (IV), wherein R is C1-C4 alkyl. The method comprises the steps: with phosphorus pentasulfide as the starting material, then carrying out vulcanization reaction, chlorination reaction, water washing and distillation purification, then carrying out catalytic hydrogenation to obtain chloride phosphite, next carrying out Grignard reaction to synthesize methyl phosphite (IV), and thus obtaining the final product glufosinate-ammonium through a Strecker route of the prior art. The synthetic yield is increased, methyl phosphorus dichloride and other unstable corrosive intermediates cannot be produced, the discharge of three-waste substances is reduced, and environment-friendly costs and pressure are reduced.
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Paragraph 0030; 0047
(2016/11/07)
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- O, O-dialkyl thiophosphoryl chloride drog-free preparation method
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The invention discloses a waste residue-free preparation method of O,O-dialkyl thiophosphoryl chloride, which is characterized by comprising the following steps: by taking dialkyl chlorophosphite as an intermediate, performing chlorination with O,O-dialkyl phosphorodithioate under the effect of strong Lewis acid metal chloride to prepare O,O-dialkyl thiophosphoryl chloride with the structural general formula shown in the specification, wherein the chemical equation is shown in the specification. The method for preparing high-content O,O-dialkyl thiophosphoryl chloride, disclosed by the invention, has the advantages of simple process route, mild reaction conditions, simple after-treatment and low production cost, and is convenient for industrial transformation; and the method avoids or reduces pollution, strictly controls the process, saves after-treatment and prevents the generation of viscose waste sulfur residues.
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Paragraph 0024; 0025
(2017/01/12)
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- Design and synthesis of novel active phosphonate esters and their application in preparation of ceftriaxone
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For a series of active phosphonate esters, the anhydride abbreviated as ANPTA (6a) exhibits the highest reactivity in the preparation of ceftriaxone. The synthesis of ceftriaxone was optimized with the pilot-scale yield reaching 95.7%. The results were explained from the structural viewpoint and supported by analysis of the calculated Mulliken atomic charge distribution.
- Ren, Hui-Xue,Sun, You-Min,Wu, Dao-Ji,Ma, Yong-Shan,Ying, Han-Jie,Ma, Yan
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p. 155 - 159
(2014/07/07)
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- An efficient synthesis of O,O- di propyl (E)-2-[1-methyl 2-oxopropylidene]phosphorohydrazidothiolate (E) oxime and its analogues: A potential marine toxin
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An efficient method for the synthesis of Ptychodiscus brevis toxin O,O- di n-propyl (E)-2-[1-methyl 2-oxopropylidene]phosphorohydrazidothiolate (E) oxime (TG-1) and its analogues has been developed using thermally stable and recyclable silica gel and Na2SO4 as a condensing agent and water scavenger, respectively. The compounds were evaluated against fish Rasbora daniconius by determining the LC50 and LC90 values. The results of biological evaluation showed that these compounds have high degree of toxicity. Copyright Taylor & Francis Group, LLC.
- Gupta, Arvind K.,Dubey,Parashar,Kaushik
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scheme or table
p. 1892 - 1910
(2009/08/07)
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- Synthesis of N-(thio)phosphoryl-N′-2-benzoxazolyl semicarbazides
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We prepared the benzoxazole derivatives bearing the (thio) phosphoryl moiety by addition reactions of 2-hydrazionbenzoxazole with isothiocyanato (thio) phosphates and characterized their structures by elementary analysis and 1H NMR and IR spectral data. From the results of biological activity screening, we found that these compounds possess some herbicidal, and plant growth regulator activities, and especially good fungicidal activity against Puccinia recondita.
- Chen, Wen-Bin,Jin, Gui-Yu
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p. 151 - 155
(2007/10/03)
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- Selective Sulfur Oxygenation in Phosphoroamidate, Thionophosphate, and Thiophosphate Agrochemicals by Perfluoro-cis-2,3-dialkyloxaziridine
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Several organophsophorus agrochemicals 2a-g with thioether, phosphoramidic, phosphorothioic, and phosphorothionic functions were reacted with perfluoro-cis-2-n-butyl-3-n-propyloxaziridine 1.The selective oxygenation of sulfide function to give sulfoxide derivatives 3a-g occured in high yields without overoxidation to sulfone products.Sulfoxides 3a-e were further oxidized under mild conditions to the corresponding sulfones 4a-e.All the products are themselves of interest as analytical environmental standards and their preparation is described in detail.
- Terreni, Marco,Pregnolato, Massimo,Resnati, Giuseppe,Benfenati, Emilio
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p. 7981 - 7992
(2007/10/02)
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- Reactions of Trico-ordinate Phosphorus Compounds with Phosphorus Pseudohalogens. Part 2. Pentaco-ordinate Intermediates in the Reaction of o-Phenylene Neopentyl Phosphite with Diethoxyoxophosphoranesulfenyl Chloride
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Reaction between oxophosphoranesulfenyl chloride 1 (R = R' = EtO) and o-phenylene neopentyl phosphite 4 takes predominantly the deoxygenation course, yielding the phosphorochloridothioate 7 and the phosphate 8.Formation of minor products 5 and 6 corresponding to the desulfurization pathway, and low-temperature 31P NMR observations, are rationalized by proposing phosphorane-phosphonium equilibria which are shifted towards phosphorane structures 9, 13, 11.These results supplement our earlier studies on desulfurization and deoxygenation of compound 1 with tricoordinate phosphorus compounds and add new evidence for phosphonium-phosphorane equilibria.
- Krawczyk, Ewa,Skowronska, Aleksandra,Michalski, Jan,Mikolajczak, Jerzy
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p. 851 - 854
(2007/10/02)
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- Reaction of Tricoordinate Phosphorus Compounds with Organophosphorus Pseudohalogens. 1. Desulfurization and Deoxygenation of Oxophosphoranesulfenyl Chlorides. Scope and Mechanism
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The reaction of oxophosphoranesulfenyl chlorides RR'P(O)SCl 2 with PIII compounds has been investigated.Its mechanistic features have been elucidated by variable-temperature 31P NMR spectroscopy and stereochemical changes at PIV and PIII phosphorus centers.These studies show that in all cases phosphonium intermediates containing the sulfur bridge >P(O)-S-P(+)P(S)-O-P(+)-Cl(-).The latter decomposes by the attack of the chloride anion on the thiophosphoryl center (deoxygenation pathway). 31P NMR studies fully corroborated the observed stereochemical changes.
- Krawczyk, E.,Mikolajczak, J.,Skowronska, A.,Michalski, J.
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p. 4963 - 4970
(2007/10/02)
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- NEW CHEMISTRY AND STEREOCHEMISTRY OF ORGANOPHOSPHORUS PSEUDOHALOGENS
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Synthesis, chemistry and stereochemistry of organophosphorus-sulfur(selenium)pseudohalogens are discussed and rationalized.
- Michalski, Jan,Skowronska, Aleksandra,Lopusinski, Andrzej
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- REACTION OF TRICOORDINATE PHOSPHORUS COMPOUNDS WITH PSEUDOHALOGENS. SCOPE AND MECHANISM
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The selectivity of sulphur, selenium and oxygen removal from pseudohalogens: phosphorus disulphides 1 and 2, diselenides 3 and oxophosphoranesulphenyl chlorides 4 has been investigated.A mechanistic rationalization is proposed to account for sulphur(selenium)/oxygen extrusion variation as a function of substrates structure and reaction conditions.
- Skowronska, Aleksandra,Krawczyk, Ewa,Burski, Janusz
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p. 233 - 236
(2007/10/02)
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- REDOX REACTIONS OF ANTIMONY(III) O,O-DISUBSTITUTED PHOSPHORODITHIOATES WITH FERRIC CHLORIDE
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The reaction of antimony(III) tris-(O,O-diethylphosphorodithioate) with three equivalents of ferric chloride in ether solution has been found to give ferrous chloride, bis-(O,O-diethylthiophosphoryl) disulfide and dichloroantimony O,O-diethyl phosphorodithioate as the major products.However, a relatively low yield of bis-(O,O-diethylthiophosphoryl) trisulfide was also obtained.The structures of these products were established by independent syntheses.Several additional antimony(III) tris-(O,O-disubstituted phosphorodithioates) were prepared, and the major organic product obtained by reaction of each of these compounds with three equiva lents of ferric chloride was the corresponding bis-(O,O-disubstituted thiophosphoryl) disulfide.A mechanism for this reaction has been suggested, and evidence in support of the mechanism has been presented.The various antimony(III) tris-(O,O-dialkyl phosphorodithioates) are passivating agents in petroleum refining.The results reported in this and in our previous papers indicate that such compounds undergo a variety of reactions with components of crude petroleum prior to the ultimate pyrolysis reactions which occur in the fluid catalytic cracking process.
- Woo, Edward J.,Kalbacher, Barbara J.,McEwen, William E.
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p. 269 - 278
(2007/10/02)
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- Participation of Anions of Dialkyl Phosphites and Thiophosphites in Aliphatic SRN1 Reactions
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Dialkyl phosphite or thiophosphite anions react with 2-chloro- or 2(p-tolylsulfonyl)-2-nitropropane, p-nitrobenzyl chloride, and α,α-dimethyl-p-nitrobenzyl chloride to form in a free radical chain process the α-nitroalkyl or p-nitrobenzyl phosphonates or thiophosphonates which may be reduced to the amino derivatives. 2,2-Dinitropropane reacts with dialkyl phosphite or dimethyl thiophosphite ions to form dialkyl phosphate or thiophosphate esters of acetone oxime.The relative reactivities of a series of anions toward Me2CNO2, p-O2NPhCH2, and p-O2NPhC(Me)2 are reported.
- Russel, Glen A.,Ros, Francisco,Hershberger, J.,Tashtoush, Hasan
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p. 1480 - 1483
(2007/10/02)
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- Synthesis and Insecticidal Activity of N4-Aryl-N1-(O,O-dialkyl thiophosphoryl)Piperazines
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Eleven new N4-aryl-N1-(O,O-dialkyl thiophosphoryl) piperazines have been synthesised as possible insecticides by the condensation of N-aryl piperazines with O,O-dialkyl chloro-tiophosphates and tested against Periplanata americana.
- Agarwal, Kamlesh C.
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p. 1170 - 1171
(2007/10/02)
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- Production of O,O-dialkyl-phosphorochloridothionates
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An O,O-dialkyl-dithiophosphoric acid ester is reacted in two steps with approximately an equimolar amount of chlorine, the first step at about 0° to 80° C with all the reactants supplied, and the second step at about 0° to 100° C with precipitation of sulfur from the disulfur dichloride which is produced as a by-product in the first step and which serves as the chlorinating agent in the second step. Advantageously the first step is carried out continuously in two stages about one-third to two-thirds of the chlorine being supplied continuously to each stage. The first stage is at about 30° to 60° C and the second stage at about 10° to 25° C. The second step is thereafter performed batchwise and the desired product is distilled off from the residual sulfur.
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