磺酰脲类除草剂噻磺隆的非光气法合成

除草剂;磺酰脲类除草剂噻磺隆的非光气法合成     

An efficient method for the synthesis of dialkyl chlorophosphates from trialkyl phosphites using bis（trichloromethyl） carbonate

A mild and simple method for the synthesis of dialkyl chlorophosphates is described, bis（trichloromethyl） carbonate （BTC） is used as the effective reagent for the conversion of dialkyl phosphites to their corresponding dialkyl chlorophosphates under mild conditions.     

A Novel Synthesis of Alkylamino Substituted Methylenediphosphonates Using Bis(trichloromethyl) Carbonate and RCONR1R2

An efficient, economical and easy method for the synthesis of dimethylaminomethylenediphosphonates using bis(trichloromethyl) carbonate and RCONR1R2 has been developed, which proceeded under relatively mild conditions.     

双（三氯甲基）碳酸酯的制备和应用

介绍了近１０年双（三氯甲基）碳酸酯（简称ＢＴＣ）的制备方法及其在有机合成中的应用。ＢＴＣ作为剧毒的光气和双光气在合成中的低毒替代物,在制备一些重要类型有机化合物时,其反应条件温和,选择性好,收率高。     

二（三氯甲基）碳酸酯替代光气合成二苯甲酮类化合物

二（三氯甲基）碳酸酯替代光气合成二苯甲酮类化合物彭孝军，颜英，周卓华（大连理工大学化工学院大连１１６０１２）关键词二苯甲酮，二（三氯甲基）碳酸酯，光气二芳甲酮类化合物是重要的精细化工产品，如二苯甲酮为紫外线吸收剂，Ｎ，Ｎ，Ｎ′，Ｎ′－四甲基米氏酮、Ｎ...     

Activation of Supports Containing Hydroxyl Groups Using bis(4-Nitrophenyl) carbonate

Abstract

The hydroxyl groups carrying supports, Sepharose Cl-4B and Fractogel HW75F, were facilely activated under anhydrous conditions using bis(4-nitrophenyl) carbonate (BPNPC), a stable and readily available compound. The activation time at room temperature can be as short as 0.5 hour. The activated supports can be stored at 4°C for at least one month without any loss of coupling capacity. Amines can be coupled to the activated support at pH 7 to 10. Coupling of Protein A to BPNPC activated supports yielded immobilized Protein A affinity supports having a high IgG binding capacity. For example, the Protein A-Sepharose and Protein A-Fractogel prepared by using the BPNPC activation method were able to bind, respectively 13 - 14 mg and 8 - 9 mg human IgG with phosphate buffer saline as the loading buffer. In contrast the use of a high yield binding buffer increases the binding capacity of the two affinity supports to 25 - 28 mg and 22 mg respectively.     

New odorless method for the Corey-Kim and Swern oxidations utilizing dodecyl methyl sulfide (Dod-S-Me)

Development of the odorless dodecyl methyl sulfide (Dod-S-Me, 1) as an alternative for dimethyl sulfide (DMS) and new odorless methods for the Corey-Kim and Swern oxidations are described. These reactions have been developed with a view toward green chemistry, utilizing Dod-S-Me (1) and common solvents instead of dichloromethane.     

Molecular structure of (3,5-diallylisocyanuratomethyl)bis(chloromethyl)phosphine oxide. Synthesis of (3,5-diallylisocyanuratomethyl)phosphine sulfides

X-Ray study of the (3,5-diallylisocyanuratomethyl)bis(chloromethyl)phosphine oxide showed that the phosphorylmethyl group is bonded to the nitrogen atom of the cycle. Reaction of the tris(chloromethyl)phosphine sulfide with sodium diallylisocyanurate gave (3,5-diallylisocyanuratomethyl)bis(chloromethyl)phosphine sulfide, and treatment of the tris(3,5-diallylisocyanuratomethyl)phosphine oxide with phosphorus pentasulfide gave a tris(3,5-diallylisocyanuratomethyl)bis(chloromethyl)phosphine sulfide.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1446–1448, August, 1993.     

Temperature-dependent dielectric studies of fully cured diethylene glycol bis (allyl carbonate)

Studies are presented of the dielectric properties of fully cured diethylene glycol bis (allyl carbonate) as a function of both frequency and temperature. It is shown that the characteristics of the fully cured system are dominated by a localized, secondary transition that is associated with motion of the carbonate unit. The glass transition is shown to contribute little to the dielectric properties within the temperature range 20–70°C. © 1994 John Wiley & Sons, Inc.     

Preparation of samarimm(ii) sulfide by the reaction of samarium(II) bis[bis(trimethylsilyl)amide] with hydrogen sulfide

X-ray amorphous samarium(II) sulfide was prepared by the reaction of H₂S with samarium(II) bis[bis(trimethylsilyl)amide] (1) in THF at 10^–2 Torr. Compound1 was prepared by two methods: 1) the reaction of SmI₂ with lithium bis(trimethylsilyl)amide and 2) the reaction of samarium naphthalide with bis(trimethylsilyl)amine. SmS was transformed to the polycrystalline state with the lattice parametera = 5.92 Å by annealing at 400–500 °C.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 241–243, February, 1995.     

An approach to synthesis of (Z)-2-chloro-1,3-diarylpropen-1-ones by Vilsmeier reagent (bis-(trichloromethyl) carbonate/DMF)

A series of(Z)-2-chloro-1,3-diarylpropen-1-ones were unexpectedly synthesized in moderate yields by treatment of easily available 2,3-epoxy-1,3-diarylpropan-1-ones with Vilsmeier reagent,which was derived from bis(trichloromethyl) carbonate(BTC, triphosgene) and DMF.A possible mechanism was also proposed,where sequential ring-opening,halogenation and elimination reactions were involved.     

亚砜还原法合成聚苯醚硫醚的结构与性能研究

以氟苯和氯化亚砜反应合成了4,4’-二氟二苯亚砜,并将其与4,4’二羟基二苯硫醚在N-甲基吡咯烷酮溶剂中进行亲核取代反应合成了聚苯醚硫醚醚亚砜,用乙二酰氯/四丁基碘化铵还原该亚砜聚合物制备了聚苯醚硫醚。用红外光谱和核磁共振谱对合成单体的结构进行了确认,同时对聚合物进行了红外光谱、核磁共振、元素分析、X射线光电子能谱、X射线衍射、DSC分析、TG/DTG以及溶解性测试。结果表明聚苯醚硫醚样品具有氧醚和硫醚交替的线性结构,特性粘度为0.55 dL/g的PPSE熔点达236℃,在氮气条件下,样品起始分解温度和最大分解速率处温度分别为359℃和514℃,在700℃时的重量保留率为43.3%,且在加热条件下能溶解于N-甲基吡咯烷酮(NMP)、二甲基乙酰胺(DMAc)、二甲基甲酰胺(DMF)等极性有机溶剂中。     

Synthesis and characterization of sodium bis(trimethylstannyl) amide and bis(trimethylsilyl) bis(trimethylstannyl) -phospha-tetrazene

Sodium bis(trimethylstannyl)amide NaN(SnMe₃)₂, isolated by the reaction of trimethylstannyldiethylamine with sodium amide, reacts with tris(trimethylsilyl)hydrazino—dichloro-phosphine to form bis(trimethylsilyl)bis(trimethylstannyl)-2-phospha-2-tetrazene, (Me₃Si)₂N-N=P-N(SnMe₃)₂. Both the molecules have been isolated and characterized.     

Bis(tetramethylammonium), bis(tetrabutylammonium), and bis(tetraphenylarsonium) dihydrohexaoxoxenonates(VIII)

Bis(tetramethylammonium), bis(tetrabutylammonium), and bis(tetraphenylarsonium) dihydrohexaoxoxenonates(VIII) were obtained in an aqueous solution and in acetonitriie. The rate constants of their decomposition were determined.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 184–185, January, 1995.This work was carried out with financial support from the International Scientific Foundation (Grant REI 000).     

液相色谱-质谱联用分析土壤中的双(2-羟乙基)亚砜

建立了液相色谱 质谱联用技术测定土壤中双(2 羟乙基)亚砜的方法。对影响检测灵敏度的流动相组成、流速、探头温度等因素进行了优化,在优化实验条件下,方法线性范围在0.05～20mg L之间,最低检测质量浓度为0.025mg L(S N>3),对比了3种萃取剂对4种土壤中的双(2 羟乙基)亚砜的萃取率,结果表明,用水作萃取剂的萃取效果最佳,回收率在92%以上,RSD均小于4%。     

Synthesis and structural studies of a bis(carbamoyl methyl) sulfoxide complex of uranyl nitrate

A new tri-functional ligand ⁱBu₂NCOCH₂SOCH₂CONⁱBu₂ was prepared and characterized. The coordination chemistry of this ligand with uranyl nitrate was studied with IR, ¹H NMR, electrospray mass–spectrometry, thermogravimetry, and elemental analysis. The structure of [UO₂(NO₃)₂(ⁱBu₂NCOCH₂SOCH₂CONⁱBu₂)] was determined by single-crystal X-ray diffraction. The uranium(VI) ion is surrounded by eight oxygens in a hexagonal bipyramidal geometry. Four oxygens from two nitrates and two oxygens from the ligand form a planar hexagon. The ligand is a bidentate chelate, bonding through sulfoxo and one of the carbamoyl groups to uranyl nitrate.     

Synthesis of novel bis(chromenes) and bis(chromeno[3,4-C]pyridine) incorporating piperazine moiety

Novel bis(2-oxo-2H-chromene) as well as bis(2-imino-2H-chromene) derivatives incorporating piperazine moiety were prepared by the cyclocondensation reaction of bis(2-hydroxybenzaldehyde) with two equivalents of each of the appropriate β-ketoesters or acetonitrile derivatives. The bis(2-imino-2H-chromene-3-carbothioamide) derivative was used as a key synthon for construction of novel bis(3-(4-substituted thiazol-2-yl)-2H-chromen-2-one) derivatives via its cyclocondensation with a series of the appropriate α-halocarbonyl derivatives. Moreover, the bis(2-hydroxybenzaldehyde) reacted with four equivalents of the appropriate acetonitrile derivatives to afford the corresponding bis(3H-chromeno[3,4-c]pyridine) derivatives. Elucidation of the structure of the novel bis(chromenes) bearing piperazine nucleus was established by the spectral data and elemental analyses.     

Polybenzoxazole from 1,4-bis(trichloromethyl)benzene

High molecular weight poly(phenylenebenzobisoxazole) (PBO) was synthesized from 1,3-diamino-4,6-dihydroxybenzene dihydrochloride (1) and 1,4-bis(trichloromethyl)benzene (3) in polyphosphoric acid (PPA) or a mixture of PPA and methanesulfonic acid. When PPA was used as the solvent, 3 was first converted in situ to terephthalic acid before 1 was added to minimize degradation of 1. Compound 3 did not need to be sealed from atmospheric moisture because the trichloromethyl groups were not moisture sensitive. It was not necessary to use micronized 3. Adjustment of P₂O₅ content was optional for this reaction because no water was liberated from the condensation of 1 and 3. © 1997 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 35 : 2143–2145, 1997     

手性亚砜法合成粉 虫性信息素

5-氯-2-戊酮(2)经四步反应制得(R)-(+)-4-甲基-3-戊烯基对甲苯基亚砜(6), 化合物6与乙醛进行不对称加成反应得手性醇(7), 7经兰尼镍还原性脱硫反应即合成出目标产物粉 虫性信息素(1), 其光学纯度可达45%。     

Selective synthesis of di(propen-1-yl)sulfone and di(propen-1-yl)sulfoxide

Convenient selective methods of synthesis of the title compounds, based on oxidation of di(propen-1-yl)sulfide with 30% H₂O₂, have been developed.Institute of Organic Chemistry, Siberian Branch, Russian Academy of Sciences, 664033 Irkutsk. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 3, pp. 675–679, March, 1992.