乙氧氟草醚及其合成中间体的物性测定与计算

含氟农药是当前国内外广受重视的新型农药。乙氧氟草醚（2-氯-4-三氟甲基苯基3’-乙氧基-4’-硝基苯基醚,Oxyfluorfen）就是一种高效、低残留、选择性好,水、旱田兼用的广谱性除草剂,该产品的研制被国家列入科研攻关项目。在实施工业化生产中,为了满足工程设计和能量计算等要求,需要提供与乙氧氟草醚相关的若干重要中间体的物性数据,     

乙氧氟草醚同分异构体杂质的分离纯化与鉴定

采用硅胶柱层析法和半制备液相色谱法对乙氧氟草醚粗品中的乙氧氟草醚同分异构体杂质进行分离制备.根据红外光谱、元素分析、质谱和核磁共振数据,推断其结构为乙氧氟草醚的同分异构体,化学名称为2-氯-1-(3-乙氧基-4-硝基苯氧基)-5-三氟甲基苯.     

2013年授权的除草剂专利(除草剂篇)

<正>乙氧氟草醚与氟乐灵二元复配制成的除草剂及其制备方法乙氧氟草醚与氟乐灵二元复配制成的除草剂及其制备方法。该除草剂质量百分比组成:乙氧氟草醚3~10%、氟乐灵10~30%,表面活性剂5~15%,乳化剂8~20%,溶剂余量。制法是:按上述质量比,将乙氧氟草醚加溶剂混合搅拌;取氟乐灵加溶剂混合     

二苯醚类除草剂乙氧氟草醚

乙氧氟草醚 (ｏｘｙｆｌｕｏｒｆｅｎ)是二苯醚类除草剂 ,国外商品名为果尔。化学名称 :2 -氯 -1 -(3 -乙氧基 -4 -硝基苯氧基 ) -4 -(三氟甲基 )苯。化学结构 :Ｆ3ＣＣｌＯＯＣ2 Ｈ5ＮＯ2乙氧氟草醚是美国罗姆 -哈斯公司开发的含氟二苯醚类除草剂。是一种高效、低毒、低残留、选择性、水旱田兼用、广谱苗前苗后触杀型除草剂。可广泛用于水稻、大豆、棉花、油菜、蔬菜、果树、森林苗圃及其它经济作物防除多种季节性阔叶杂草和禾本科杂草。1　理化性质乙氧氟草醚原药外观为淡黄色至红褐色固体 ,相对密度 1 .4 9(2 5℃ ) ,沸点 (2 50～ 3 0 0 …     

双(4-氟苯基)苯基氧膦磺酸钠盐的合成及表征

以双(4-氟苯基)苯基氧膦为起始原料,20%发烟硫酸为磺化试剂,分别合成了双(3-磺酸钠-4-氟苯基)-3’-磺酸钠苯基氧膦、4-氟苯基-(3’-磺酸钠-4’-氟苯基)-3″-磺酸钠苯基氧膦和双(4-氟苯基)-3’-磺酸钠苯基氧膦等3种单体,实验方法操作简便、反应后处理简单且收率较高,适用于产品的大规模制备。     

生姜田杂草防除试验

将33%二甲戊乐灵EC、24%乙氧氟草醚EC和20%二甲戊·乙氧氟草醚EC用作生姜田播后苗前土壤处理,结果表明,生姜田除草20%二甲戊·乙氧氟草醚EC2400～2850ml/hm2(制剂含量)防治效果最佳,优于33%二甲戊乐灵EC和24%乙氧氟草醚EC,在推荐剂量下,对生姜安全,且有显著增产效果。     

吡唑-4-基烷基酮衍生物的合成、结构和除草活性

原卟啉原氧化酶(protox)最近被证实是已知光动力作用除草剂化合物的靶标。如许多其他除草剂的结合位置一样,原卟啉原氧化酶是几种化学结构上三级交叉类型的除草剂(图1)的酶靶标,包括二苯基醚类[如乙氧氟草醚(Oxyfluorfen),Ⅰa;三氟羧草醚(acifluorfen),Ⅰb]、噁二唑类[如噁草酮(Oxadiazon)、吡啶衍生物类(如LS82-556,(S)-2,6-二甲基-N-(α-甲基苄基)-5-丙酰基烟酰胺];吡唑-4-腈类[如M&B39279,5-氨基-1-(2,6-二氯-4-三氟甲基)苯基吡唑-4-腈,Ⅱa]和推测可能是吡唑-4-腈的类似物(如Ⅲa,表1)。可以认     

气相色谱法定量分析44%戊·氧·乙草胺乳油

采用气相色谱法定量分析44%戊·氧·乙草胺乳油中三种组分二甲戊灵、乙草胺和乙氧氟草醚的含量,分析结果表明,复配制剂中二甲戊灵、乙草胺和乙氧氟草醚的标准偏差分别0.12%,0.12%和0.087%。变异系数为0.69%,0.54%和1.71%,二甲戊灵的平均回收率为99.19%,乙草胺平均回收率为99.11%,乙氧氟草醚平均回收率为98.88%。线性关系良好。     

利用QuEChERS-超高效液相色谱串联质谱法测定姜和土壤中乙氧氟草醚残留

[目的]建立测定姜和土壤中乙氧氟草醚残留的QuEChERS-超高效液相色谱串联质谱(UPLC/MS/MS)方法,通过田间试验研究了乙氧氟草醚在姜田中的残留及消解动态。[方法]样品经乙腈涡旋提取5 min,上清液加入含PSA+C18填料的小离心管中,涡旋、离心净化后,采用UPLC/MS/MS测定。[结果]在0.001~0.5 mg/L范围内,乙氧氟草醚的进样质量浓度与其对应的峰面积间呈良好的线性关系,相关系数r=0.9999,该方法检出限(LOD)为0.001 mg/kg,最低检出质量分数(LOQ)为0.01 mg/kg。在0.01、0.05、0.1 mg/kg的添加水平下,乙氧氟草醚在姜中的平均回收率为82.0%~99.0%,相对标准偏差为5.04%~15.70%;在0.02、0.05、0.2 mg/kg的添加水平下,乙氧氟草醚在土壤中的平均回收率为90.1%~97.1%;相对标准偏差为1.95%~6.20%。[结论]乙氧氟草醚在土壤中的半衰期20.4~25.7 d;24%乙氧氟草醚乳油分别按照有效成分180、270 g a.i./hm2剂量于姜播后苗前开始施药,施药1次,姜收获时采样测定,乙氧氟草醚在姜中的残留量0.01~0.0124 mg/kg,均小于欧盟规定的最大残留限量(MRL)0.05 mg/kg,因此,在姜田中使用乙氧氟草醚,有效剂量为180 g a.i./hm2,施药1次时,不会造成其在姜中残留超标的风险。     

乙氧氟草醚防除稻田杂草效果试验

为了探索二苯醚类除草剂乙氧氟草醚在水稻田除草效果、剂量和安全性,以便经济、有效地推广使用,1991年我们用此药进行防除水稻田杂草。现将结果报道如下。一、试验材料和方法1.供试药剂:23.5%乙氧氟草醚乳油(美国罗姆-哈斯公司生产);50%丁草胺乳油     

阴离子碳菁染料的合成与聚集动力学研究

自从１９３８年，Ｓｃｈｅｉｂｅ［１］发现了菁染料聚集体中的能量传递现象，人们对菁染料的聚集行为展开了大量的研究［２，３］．由于菁染料聚集体对乳剂具有特殊的增感作用，人们主要研究聚集体在乳剂中的增感机理［４，５］以及菁染料聚集的溶剂效应与浓度效应［６］...     

Aggregation phenomena of amphiphilic UVB absorptive oligoesters containing p‐alkoxycinnamate and poly(ethylene oxide) blocks

The synthesis of new amphiphilic oligoesters containing a hydrophobic block based on p‐alkoxycinnamate and hydrophilic poly(ethylene oxide) is reported. Two hydrophobic monomers, 1,2‐(bis(4‐(2‐carboxyvinyl)phenoxy))ethane ( M2 ) and 1,12‐(bis(4‐(2‐carboxyvinyl) phenoxy))dodecane ( M12 ), were synthesized. Four oligoesters, poly((1,2‐(bis(4‐(2‐carboxyvinyl)phenoxy))ethane) ‐co‐(poly(ethylene oxide)200)) ( P2‐200 ), poly((1,2‐(bis(4‐(2‐carboxyvinyl)phenoxy))ethane)‐co‐(poly(ethylene oxide) 400)) ( P2‐400 ), poly((1,12‐(bis(4‐(2‐carboxyvinyl)phenoxy)) dodecane)‐co‐(poly(ethylene oxide)400)) ( P12‐400 ), and poly((1,12‐(bis(4‐(2‐carboxyvinyl)phenoxy))dodecane)‐co‐ (poly(ethylene oxide)1000)) ( P12‐1000 ) were then constructed by reacting the M2 or M12 with poly(ethylene oxide) (PEO) with lengths of ～ 4 (PEO 200), ～ 10 (PEO 400), or ～ 23 (PEO1000) units using multiple esterifications. These oligoesters possess UVB absorption properties and show good solubility in various organic solvents. Self‐assembly of the oligoesters into aqueous spherical colloids could be induced through an acetone to water solvent displacement technique. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Film studies of certain new aromatic–aliphatic polyamides

Two new aromatic–aliphatic polyamides containing azo linkage in the main chain based on 2,2′‐dimethyl‐4,4′‐diaminoazobenzene and adipic/2‐chloro‐5‐methyl‐1,2‐dioic acid (α‐chloro‐δ‐methyl adipic acid) were synthesized and analyzed by thermogravimetry and films were cast. Also three polymers obtained from condensation of 4,4′‐azodibenzoic acid/adipic acid and 2,2′‐bis [4‐(p‐amino phenoxy) phenyl] propane/4,4′‐diaminoazobenzene were studied in terms of mechanical and morphological properties. Film studies were carried out interms of tensile property, scanning electron microscope, dielectric, microwave, and X‐ray diffraction pattern. Thermal studies have been done using thermogravimetric analysis, differential thermal analysis, and pyrolysis‐mass spectral data. The results were correlated with structure and orientation of the molecules. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 1305–1316, 2004     

一种SGLT-2抑制齐UErtugliflozin关键中间体的简便合成

报道了一种以2-氯-5-溴苯甲酸为底物经酰化，还原，甲酰化等多步反应得到4-氯-3-（4一乙氧基苄基）苯甲醛的简便合成，提供了一种SGLT-2抑制剂Ertuglitlozin关键中间体的新合成方法，该方法所用原料和试剂廉价易得，合成路线简洁，操作简便，收率高，有利降低生产成本，提高生产效率。     

Synthesis and characterization of novel poly(amide-ether)s bearing imidazole pendants: study of physical and optical properties

Two new para-linked diether-diamines, bis(4-(4-amino-2-(4,5-diphenyl-1H-imidazol-2-yl)phenoxy) phenyl)methanone and bis(4-(4-amino-2-(4,5-diphenyl-1H-imidazol-2-yl)phenoxy) phenyl)hexafluoropropane, bearing two ortho-linked phenyl-substituted imidazole pendants and trifluoromethyl groups were synthesized by the nucleophilic chlorodisplacement reaction of the synthesized 2-(2-chloro-5-nitrophenyl)-4,5-diphenyl-1H-imidazole with 4,4′-dihydroxybenzophenone or 4,4′-(hexafluoroisopropylidene)diphenol in refluxing DMAc in the presence of potassium carbonate. These diamines were utilized to prepare a series of novel poly(amide-ether)s (PAEs) via direct phosphorylation polycondensation with aliphatic and aromatic dicarboxylic acids. The polymeric samples were readily soluble in a variety of organic solvents and formed low-colored and flexible thin films via solution casting. These polymers showed glass-transition temperatures (T _gs) between 204 and 308 °C. Thermal behaviors of the PAEs were characterized by thermogravimetric analysis, and the 10 % weight loss temperatures were found to be in the range of 330–450 °C in N₂. The PAEs exhibited fluorescence emission in solution and in solid state with maxima around 423–494 nm and with the quantum yields in the range of 6–28 %.     

Synthesis of fluorinated polyimides and their application to passive optical waveguides

Fluorinated and chlorofluorinated polyimides with high thermal stability and low optical absorption loss in the optical communication wavelengths of 1.3 and 1.55 μm were investigated for low‐loss passive waveguide applications. These polyimides were prepared from pyromellitic dianhydride (PMDA) with 1,4‐bis‐[4‐amino‐2‐(trifluoromethyl)phenoxy]tetrafluorobenzene (ATPT), 1,4‐bis‐[4‐amino‐2‐(trifluoromethyl)phenoxy]benzene (ATPB), and 1,3‐bis‐[4‐amino‐2‐(trifluoromethyl)phenoxy]‐4,6‐dichlorobenzene (ATPD). Control of the refractive indices of the polymers was achieved from 1.5397–1.5671 for TE polarization and 1.5239–1.5513 for TM polarization at 1.55 μm by copolymerization of PMDA/ATPT and PMDA/ATPB. As the amount of PMDA/ATPT was increased, the refractive indices of the polymers were decreased. Rib‐type optical waveguides were fabricated using these fluorinated polyimides. These waveguides exhibited a low propagation loss of less than 0.5 dB/cm at 1.55 μm. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 2172–2177, 2000     

Clay-reinforced semi-aromatic polyether-amide nanocomposites containing phosphine oxide moieties: synthesis and characterization

Semi-aromatic flame retardant polyether-amide/organoclay nanocomposites were synthesis through solution blending technique. Surface modification of the montmorillonite clay was performed with 1,4-bis[4,4′-amino phenoxy]butane for ample compatibilization with the polyamide matrix. The polymer chains were produced from the poly condensation reaction of bis(3-amino phenyl)phenyl phosphine oxide (4) with 1,4-(4-carboxy phenoxy)butane (3). The effect of clay dispersion and the interaction between clay and polyamide chains on the properties of nanocomposites were investigated using X-ray diffraction, scanning electron microscopy, limited oxygen index, differential scanning calorimetry, thermogravimetric analysis, and water uptake measurements. The diacid 3 as a monomer was prepared from the reaction of 4-hydroxy benzoic acid (1) with 1,4-dibromo butane (2) in the presence of NaOH solution.     

含不同阻燃元素的阻燃剂对聚丙烯阻燃性能的影响

合成一种聚苯氧基膦胍(PPPG)阻燃剂,将这种含阻燃元素磷和氮的阻燃剂和另外两种含溴阻燃剂BA—59P和PO—64P分别用于制备阻燃聚丙烯。结果表明,单独使用上述阻燃剂时,PPPG的阻燃效果比BA—59P和PO—64P为好。     

Synthesis and properties of new poly(amide‐imide)s based on 1,3‐bis[4,4'‐(trimellitimido) phenoxy] propane and aromatic diamines

Six new poly(amide‐imide)s 8a–f containing trimethylene moiety in the main chain were synthesized by the polycondensation reactions of 1,3‐bis[4,4'‐(trimellitimido) phenoxy] propane 6 with six different aromatic diamines 7a–f in a medium constituting N‐methyl‐2‐pyrrolidone, triphenylphosphite, CaCl₂, and pyridine as condensing agents. The polycondensation reaction produced a series of novel poly(amide‐imide)s 8a–f in high yields with inherent viscosities between 0.35 and 0.63 dL/g. The resulting poly(amide‐imide)s were characterized by elemental analysis, viscosity measurements, thermal gravimetric analysis (TGA and DTG), solubility tests, and FTIR spectroscopy. 1,3‐Bis[4,4'‐(trimellitimido) phenoxy] propane 6 as a new monomer containing trimethylene moiety was synthesized using a three‐step reaction. At first 1,3‐bis[4,4'‐nitrophenoxy] propane 3 was prepared by the reaction of 4‐nitrophenol 1 with 1,3‐dibromo propane 2 in DMF solution . Then, dinitro 3 was reduced to 1,3‐bis[4,4'‐aminophenoxy] propane 4 by using a solution of sodium sulfite in ethanol. Finally, 1,3‐bis[4,4'‐(trimellitimido) phenoxy] propane 6 was prepared by the reaction of one equivalent diamine 4 with two equivalents of trimellitic anhydride 5 in a mixture of acetic acid‐pyridine (3 : 2). © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010