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Silica-supported 1,3-dichloro-5,5-dimethylhydantoin(DCH) as a useful reagent for microwave-assisted aromatization of 1,3,5-trisubstituted pyrazolines under solvent-free conditions 被引量:2
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作者 Davood Azarifar Elahe Nadimi Mohammd Mehdi Ghanbari 《Chinese Chemical Letters》 SCIE CAS CSCD 2011年第4期447-450,共4页
1,3,5-Trisubstituted pyrazolines are rapidly and conveniently oxidized to their corresponding pyrazoles by 1,3-dichloro-5,5- dimethylhydantoin(DCH) in solution and solvent-free conditions under microwave irradiation... 1,3,5-Trisubstituted pyrazolines are rapidly and conveniently oxidized to their corresponding pyrazoles by 1,3-dichloro-5,5- dimethylhydantoin(DCH) in solution and solvent-free conditions under microwave irradiation.The presence of silica gel as a supporting agent is shown to be effective in reducing the reaction times and increasing the yields. 展开更多
关键词 PYRAZOLINES 1 3-dichloro-5 5-dimethylhydantoin(DCH) AROMATIZATION SOLID-SURFACE Microwave irradiation
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Soil-Air Partitioning of Polychlorinated Biphenyls and Total Dichloro-Diphenyl-Trichloroethanes 被引量:1
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作者 Yaping Zhang Erping Bi Honghan Chen 《Journal of Earth Science》 SCIE CAS CSCD 2014年第4期741-748,共8页
Soil-air partitioning is an important diffusive process that affects the environmental fate of organic compounds and human health. In this review, factors affecting the soil-air partitioning of polychlorinated bipheny... Soil-air partitioning is an important diffusive process that affects the environmental fate of organic compounds and human health. In this review, factors affecting the soil-air partitioning of polychlorinated biphenyls (PCBs) and total dichloro-diphenyl-trichloroethanes (p,p'- and o,p'- isomers of DDT, DDD, and DDE) are discussed. Hydrophobicity is an important factor that influences soil-air partition coefficients (KsA), and its effect can be explained through enthalpy of phase change for soil-air partitioning transfer (AHsA). For more hydrophobic compounds, a sharp increase in the KSA of PCBs and organochlorines can be seen in the early aging period. During the aging period, the temperature has a significant effect on the more hydrophobic organic compounds. The content and properties of soil or- ganic matter influence the KSA of the target compounds. Generally, KSA decreases with increasing rela- tive humidity in soils. The linear trend between KSA and temperature (T) changes at 0 ~C. Freezing the air or soil in experiments would change the research results. On the basis of factors influencing soil-air partitioning, a multipleparameter (T, organic carbon fraction (foe), and octanol-air partition coefficient (KoA)) model is put forward to predict the KSA values for PCBs and total DDTs. 展开更多
关键词 soil-air interface PARTITION SORPTION polychlorinated biphenyl (PCB) dichloro-diphenyltrichloroethanes (DDT).
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Synthesis of Some New Derivatives of 1,3-Dichloro-1,1,3,3-tetraphenyldisilazane
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作者 Cai Hong XU Zhi Jie ZHANG +2 位作者 Yong Min LI Zhi Min ZHENG Ze Min XIE 《Chinese Chemical Letters》 SCIE CAS CSCD 2001年第1期35-38,共4页
The reactive properties of 1,3-dichloro-1,1,3,3-tetraphenyldisilazane (DCTPS) with water, methanol, phenylamine and lithium salt of hexamethylcyclotrisilazane (D-3(NLi)) were investigated, and four new derivatives wer... The reactive properties of 1,3-dichloro-1,1,3,3-tetraphenyldisilazane (DCTPS) with water, methanol, phenylamine and lithium salt of hexamethylcyclotrisilazane (D-3(NLi)) were investigated, and four new derivatives were obtained. 展开更多
关键词 1 3-dichloro-1 1 3 3-tetraphenyldisilazane DERIVATIVES reactive properties
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Synthesis and Crystal Structure of (3,6-Dichloro-2-nitrophenyl)(3-nitrophenyl)methanone
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作者 BAI Fang GAO Guo-wei WANG Yang MEN Jian 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2011年第3期422-425,共4页
Novel compounds, (3,6-dichloro-2-nitrophenyl)(3-nitrophenyl)methanone(2), (2-amino-3,6-dichloro- phenyl)(3-aminophenyl)methanone(3) and 1-[3-(2-amino-3,6-dichlorobenzoyl)phenyl]-1H-pyrrole-2,5-dione(4)... Novel compounds, (3,6-dichloro-2-nitrophenyl)(3-nitrophenyl)methanone(2), (2-amino-3,6-dichloro- phenyl)(3-aminophenyl)methanone(3) and 1-[3-(2-amino-3,6-dichlorobenzoyl)phenyl]-1H-pyrrole-2,5-dione(4), were synthesized from the initial compound 2,5-dichlorobenzophenone(1) and characterized by 1H NMR, 13C NMR, IR, mass spectrum and element analysis, respectively. The single crystal of compound 2 was obtained and determined by X-ray diffraction analysis. The single crystal data illustrates that it belongs to the monoclinic system, space group P21/c with a=0.7587(4) nm, b=2.4724(4) nm, c=0.8081(3) nm, α=90°, β=112.85(2)°, γ=90o, V=1.3970(9) nm3, Z=4, Dc=1.622 g/cm3, Mr(C13H6Cl2N2O5)=341.10, μ(Mo Kα)=0.49 mm?1, F(000)=688, the final R=0.048 and wR=0.144 for 1665 observed reflections with I2σ(I). The title molecule forms a "T" type crystal structure and the dihedral angel of the two phenyl rings is 65.0(1)°. 展开更多
关键词 (3 6-dichloro-2-nitrophenyl)(3-nitrophenyl)methanone Crystal structure MALEIMIDE
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Synthesis of Intermediate 2, 3-Dichloro-1,4-naphthoenone for Fungicide Dithianon
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作者 Zhang Zhenming LU Liangzhong +4 位作者 Kong Xianbin Wang Jianrong Wang Gang Liu Kai Wang Xiaohui 《Plant Diseases and Pests》 CAS 2019年第1期33-36,共4页
The synthetic method of dithianon intermediate 2,3-dichloro-1,4-naphthoquinone was introduced. Starting with raw material sodium 4-amino1-naphthalene sulfonate, 2,3-dichloro-1,4-naphthoquinone was synthesized through ... The synthetic method of dithianon intermediate 2,3-dichloro-1,4-naphthoquinone was introduced. Starting with raw material sodium 4-amino1-naphthalene sulfonate, 2,3-dichloro-1,4-naphthoquinone was synthesized through acidification, chlorination and oxidation. After filtration and recrystallization, more than 98% of 2,3-dichloro-1,4-naphthoquinone was obtained, and the yield reached 76%(measured by sodium 4-amino-1-naphthalene sulfonate). 展开更多
关键词 FUNGICIDE Dithianon 2 3-dichloro-1 4-naphthoquinone Synthesis
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A New Technique for Synthesis of 2,4-Dichloro-Thieno[3,2-d]Pyrimidine
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作者 DONG Liuyu GUI Houying +2 位作者 ZHOU Qiuming HU Xinming GUI Shaoyong 《Wuhan University Journal of Natural Sciences》 CAS 2012年第2期177-184,共8页
3-Amino-2-methoxycarbonylthiophene used as the main raw material,an intermediate(thiofuran siamese) 2,4-dichloro-thieno[3,2-d]pyrimidine was synthesized.The prod-uct was characterized by nuclear magnetic resonance(... 3-Amino-2-methoxycarbonylthiophene used as the main raw material,an intermediate(thiofuran siamese) 2,4-dichloro-thieno[3,2-d]pyrimidine was synthesized.The prod-uct was characterized by nuclear magnetic resonance(NMR).The first step yield was 84%(190 ℃) and the second step yield was 81.4%(105 ℃,m(intermediate):m(phosphorus oxychloride) = 1:6.4).The raw product was refined with a unique refining process,which can enhance the purity up to 99.5% to meet the requirement of condi-tions for the development and research of thiofuran siamese as a new medicine of anticarcinogen.Contrasted with the traditional technique,this process featured with cheap raw materials,possible for solvent recovery and reuse,low comprehensive cost,and suit-able for production on certain scale. 展开更多
关键词 3-amino-2-methoxycarbonylthiophene antitumor 2 4-dichloro-thieno[3 2-d]pyrimidine
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Enantioselective Chlorocyclization of Olefinic Amides with 1,3-Dichloro-5,5-Dimethylhydantoin(DCDMH) Catalyzed by(DHQD)2PHAL
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作者 ZHOU Qingjun GUO Chao +3 位作者 LI Xiwang HE Pei YANG Guichun DONG Chune 《Wuhan University Journal of Natural Sciences》 CAS CSCD 2018年第3期259-264,共6页
An efficient catalytic asymmetric chlorocyclization of olefinic amides with 1,3-dichloro-5,5-dimethylhydantoin(DCDMH) using hydroquinidine 1,4-phthalazinediyl diether((DHQD)_2 PHAL) as organocatalyst has been de... An efficient catalytic asymmetric chlorocyclization of olefinic amides with 1,3-dichloro-5,5-dimethylhydantoin(DCDMH) using hydroquinidine 1,4-phthalazinediyl diether((DHQD)_2 PHAL) as organocatalyst has been developed. Series of chiral chloro substituted isobenzofuran-1(3 H)-imine derivatives were obtained in good yields(up to 85%) and enantioselectivities(up to 70% ee). 展开更多
关键词 Catalyzed by Dimethylhydantoin Enantioselective Chlorocyclization of Olefinic Amides with 1 3-dichloro-5 DCDMH
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Microwave Synthesis and Crystal Structure of Bis{2-[(2,4-dichloro-phenylimino)methyl]-4,6-diiodo-phenol}-copper(Ⅱ)
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作者 徐锁平 阮班锋 +1 位作者 裴元 朱海亮 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2012年第10期1391-1394,共4页
Bis{2-[(2,4-dichloro-phenytimino)-methyl]-4,6-diiodo-phenol}-copper(II) (1) has been synthesized and its structure determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n wit... Bis{2-[(2,4-dichloro-phenytimino)-methyl]-4,6-diiodo-phenol}-copper(II) (1) has been synthesized and its structure determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n with a = 14.7558(17), b = 20.770(2), c = 20.3260(19) A, β = 90.6110(10)°, V= 6229.2(11) A3 and Z = 8. The Cu atom is surrounded by two O atoms and two N atoms from two 2-[(2,4-diehloro-phenylimino)-methyl]-4,6-diiodo-phenol molecules to form a tetrahedral coordination environment. The complex is linked into a column by weak intermolecular interactions. 展开更多
关键词 copper complex microwave synthesis crystal structure 2-[(2 4-dichloro-phenyl-imino)-methyi]-4 6-diiodo-phenol
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气相色谱-串联质谱法测定白芍中滴滴涕的不确定度评定
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作者 颜梅 何钦 《中华中医药学刊》 北大核心 2026年第2期230-233,共4页
对气相色谱-串联质谱法(GC-MS/MS)测定白芍中禁用的滴滴涕(DDT)残留量的不确定度进行评定,参考《中华人民共和国药典》(2020版)“药材及饮片(植物类)中禁用农药多残留测定方法”,建立测量数学模型,对不确定度来源进行分析,包括标准溶液... 对气相色谱-串联质谱法(GC-MS/MS)测定白芍中禁用的滴滴涕(DDT)残留量的不确定度进行评定,参考《中华人民共和国药典》(2020版)“药材及饮片(植物类)中禁用农药多残留测定方法”,建立测量数学模型,对不确定度来源进行分析,包括标准溶液配制、样品制备、测量重复性、标准曲线、气相色谱-串联质谱仪、回收率。通过计算各个不确定度分量并合成,得到4,4'-滴滴伊(4,4'-DDE)、2,4'-滴滴涕(2,4'-DDT)、4,4'-滴滴滴(4,4'-DDD)、4,4'-滴滴涕(4,4'-DDT)的结果可分别报告为(0.14±0.01)、(0.13±0.01)、(0.14±0.01)、(0.13±0.03)mg·kg^(-1),(k=2)。测定结果的不确定度主要受标准曲线拟合、标准溶液配制的因素影响。 展开更多
关键词 气相色谱-串联质谱法 不确定度评定 白芍 禁用农药 滴滴涕
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PROPERTIES AND APPLICATION OF THE HERBICIDE N-3′,4′-DICHLORO-α-METHYL-PROPIONANILIDE
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作者 张宗涛 武义森 《Chinese Science Bulletin》 SCIE EI CAS 1981年第2期192-,共1页
The amide herbicide has been studied systematically in our laboratory for many years. We have synthesized 74 kinds of amide-compounds, most of which are aliphatic amides and the others are furfural and aromatic amides... The amide herbicide has been studied systematically in our laboratory for many years. We have synthesized 74 kinds of amide-compounds, most of which are aliphatic amides and the others are furfural and aromatic amides. It has been found that the N-3′, 4′-dichloro-α-methyl-propionanilide (DCMPA) behaves as effective as N-3.4-dichloro- 展开更多
关键词 dichloro systematically AMIDE AROMATIC dichloro 沙七 刃刀 田劝 生七 日印
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气相色谱-串联质谱法测定食品接触用纸制品中2种氯丙醇的残留量及其释放规律探讨 被引量:2
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作者 韩陈 吴亚平 孙多志 《理化检验(化学分册)》 北大核心 2025年第7期824-829,共6页
将食品接触用纸制品裁剪成约1 cm^(2)的小块,取10 g样品置于具塞三角烧瓶中,加入200 mL沸水,于80℃加热2 h,冷却后,用水定容至250 mL。取5.00 mL上述溶液置于试管中,加入0.05 mL 10 mg·L^(−1)混合内标溶液和1 g氯化钠,溶解后过硅... 将食品接触用纸制品裁剪成约1 cm^(2)的小块,取10 g样品置于具塞三角烧瓶中,加入200 mL沸水,于80℃加热2 h,冷却后,用水定容至250 mL。取5.00 mL上述溶液置于试管中,加入0.05 mL 10 mg·L^(−1)混合内标溶液和1 g氯化钠,溶解后过硅藻土固相萃取小柱,平衡10 min,用18 mL乙酸乙酯洗脱,收集洗脱液,加入4 g无水硫酸钠,静置10 min,过滤。收集过滤液,于45℃氮吹至近干,加入2 mL正己烷溶解,快速加入0.04 mL七氟丁酰基咪唑,涡旋30 s,于70℃电热鼓风干燥箱中衍生30 min。冷却至室温,加入20%(质量分数)氯化钠溶液2 mL,涡旋1 min,静置分层,取上层溶液,加入0.3 g无水硫酸钠干燥,过0.22μm尼龙滤膜,采用气相色谱-串联质谱法测定滤液中2种氯丙醇[1,3-二氯-2-丙醇(1,3-DCP)、3-氯-1,2-丙二醇(3-MCPD)]的含量。2种氯丙醇的衍生物在SH-Rxi-5Sil MS色谱柱上按照柱升温程序分离,采用电子轰击离子源以多反应监测模式检测,同位素内标法定量。结果表明,2种氯丙醇的质量浓度均在0.5~200.0μg·L^(−1)内与其内标质量浓度的比值和对应的衍生物峰面积与内标衍生物峰面积比值呈线性关系,检出限(3S/N)均为0.25μg·L^(−1)。按照标准加入法进行回收试验,回收率为80.9%~116%,测定值的相对标准偏差(n=7)为0.58%~0.85%。方法用于分析20批食品接触用纸制品样品,1,3-DCP和3-MCPD均被检出,检出量分别为2.0~16μg·L^(−1),2.0~69μg·L^(−1);此外,接触食品温度越高、接触食品时间越长,食品接触用纸制品中1,3-DCP和3-MCPD的释放量越高。 展开更多
关键词 气相色谱-串联质谱法 食品接触用纸制品 1 3-二氯-2-丙醇(1 3-DCP) 3-氯-1 2-丙二醇(3-MCPD) 衍生化
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苦基氯合成副产物1,2-二氯-3,5-二硝基苯的反应机理
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作者 崔杨瑞 张紫薇 +2 位作者 翟连杰 陆明 许元刚 《火炸药学报》 北大核心 2025年第12期1103-1109,I0001,共8页
为了研究苦基氯硝化过程中副产物1,2-二氯-3,5-二硝基苯的反应机理,探究了盐酸气通入时长、混酸体积比例(发烟硫酸/发烟硝酸)、原料1-氯-2,4-二硝基苯的质量、硝化温度等关键工艺参数对副产物质量浓度的影响;借助液相色谱检测跟踪其浓... 为了研究苦基氯硝化过程中副产物1,2-二氯-3,5-二硝基苯的反应机理,探究了盐酸气通入时长、混酸体积比例(发烟硫酸/发烟硝酸)、原料1-氯-2,4-二硝基苯的质量、硝化温度等关键工艺参数对副产物质量浓度的影响;借助液相色谱检测跟踪其浓度变化情况。结果表明,当盐酸气通入时间为3 h、混酸体积比为5∶1、原料质量为1.0 g、硝化温度控制在130℃时,此时副产物的质量浓度最高;随着硝化反应后期发烟硝酸浓度降低,过剩发烟硫酸与原料中氯离子反应,在强酸中经均裂产生Cl·自由基或与H^(+)结合形成Cl^(+)等价物种参与亲电取代,促进了副产物1,2-二氯-3,5-二硝基苯的形成;延长硝化时间,控制混酸体积比和硝化温度、避免HCl通气可有效抑制副产物生成,提升苦基氯纯度达到95%及以上。 展开更多
关键词 有机化学 苦基氯 1 2-二氯-3 5-二硝基苯 硝化 耐热炸药 LLM-126
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Aspects on the Mechanism of the 1-Phenyl-1<i>H</i>-pyrazolo[3,4-<i>b</i>]quinoxaline Formation 被引量:1
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作者 Mohamed A. Mostafa Salah L. Aboulela +2 位作者 Mohammed A. E. Sallam Farida F. Louis Thorleif Anthonsen 《Green and Sustainable Chemistry》 2012年第2期71-75,共5页
Condensation of D-glucose, o-phenylenediamine and N,N-benzylphenylhydrazine hydrochloride (NNBPHH) in a one-pot reaction, or condensation of 2-(D-arabino-tetritol-1-yl) quinoxaline and NNBPHH, gave 3-(D-erythro-glycer... Condensation of D-glucose, o-phenylenediamine and N,N-benzylphenylhydrazine hydrochloride (NNBPHH) in a one-pot reaction, or condensation of 2-(D-arabino-tetritol-1-yl) quinoxaline and NNBPHH, gave 3-(D-erythro-glycerol-1- yl)-1-phenyl-1H-pyrazolo[3,4-b]quinoxaline. The structure of the latter was determined by 1H NMR spectroscopy and by synthesis using phenylhydrazine hydrochloride instead of NNBPHH. Condensation of D-glucose and 4,5-dichloro-o-phenylenediamine gave 6,7-dichloro-2-(D-arabino-tetritol-1-yl)quinoxaline, which upon condensation with NNBPHH gave the corresponding 6,7-dichloro-3-(D-erythro-glycerol-1-yl)-1-phenyl-1H-pyrazolo[3,4-b]quinoxaline. The structure and mechanism of formation of these compounds are discussed. 展开更多
关键词 2-(D-arabino-tetritol-1-yl)quinoxaline Pyrazolo[3 4-b]quinoxalines 3-(D-erythro-glycerol-1-yl)-1-phenyl-1H-pyrazolo-[3 4-b]qunoxaline 4 5-dichloro-o-phenylenediamine 6 7-dichloro-2-(D-arabino-tetritol-1-yl)quinoxaline 7-dichloro-3-(D-erythro-glycerol-1-yl)-1-phenyl-1H-pyrazolo-[3 4-b]quinoxaline N N-Benzylphenylhydrazine hydrochloride
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一种五甲基环戊二烯二氯合钌(Ⅲ)聚合物的批量制备方法
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作者 李天赐 黄光英 +1 位作者 姚默鎏昕 晏彩芬 《贵金属》 北大核心 2025年第S1期204-208,共5页
本研究以水合三氯化钌和五甲基环戊二烯为原料,甲醇为溶剂,经搅拌反应、过滤、洗涤、干燥等操作,高效合成五甲基环戊二烯二氯合钌(Ⅲ)聚合物,产率为85.23%。对产品进行的表征证明得到了目标产物。该制备方法操作简便,产率较高,可实现批... 本研究以水合三氯化钌和五甲基环戊二烯为原料,甲醇为溶剂,经搅拌反应、过滤、洗涤、干燥等操作,高效合成五甲基环戊二烯二氯合钌(Ⅲ)聚合物,产率为85.23%。对产品进行的表征证明得到了目标产物。该制备方法操作简便,产率较高,可实现批量化制备生产。 展开更多
关键词 五甲基环戊二烯二氯合钌聚合物 批量制备 合成
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2,2-二氯-1,1,1-三氟乙烷的制备研究进展
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作者 王军祥 孙彦波 +2 位作者 赵胜 程吉锋 周征一 《浙江化工》 2025年第8期9-16,共8页
2,2-二氯-1,1,1-三氟乙烷(HCFC-123)是重要的氢氯氟烃(HCFCs)化合物,在制冷、发泡剂等行业中具有重要应用。由于其较低的消耗臭氧潜能值和优良的热力学性能,HCFC-123被广泛用作氯氟烃(CFCs)的替代品,尤其在离心式冷水机组和高温热泵等... 2,2-二氯-1,1,1-三氟乙烷(HCFC-123)是重要的氢氯氟烃(HCFCs)化合物,在制冷、发泡剂等行业中具有重要应用。由于其较低的消耗臭氧潜能值和优良的热力学性能,HCFC-123被广泛用作氯氟烃(CFCs)的替代品,尤其在离心式冷水机组和高温热泵等领域表现出优异的适用性。近年来,随着环保法规的日益严格和行业需求的增长,开发高效、经济的HCFC-123合成工艺具有重要意义。本文系统梳理了HCFC-123的主要制备方法,基于不同原料路线和关键工艺进行分类,并对比分析了各技术路线的优缺点及工业化可行性,以期为相关领域的研究与生产提供参考。 展开更多
关键词 2 2-二氯-1 1 1-三氟乙烷 制备 催化剂
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二氯喹啉酸的绿色制备工艺研究
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作者 李炜 吴春辉 《精细石油化工》 2025年第6期23-25,共3页
报道了一种基于Cu-Co-Ru三元复合催化剂的二氯喹啉酸绿色合成工艺。以3,7-二氯-8-二氯甲基喹啉(M2)作原料,双氧水作氧化剂,通过优化催化剂组成、反应温度等控制条件,显著提高了反应效率和环境友好性。实验结果表明:催化剂总量为底物M2... 报道了一种基于Cu-Co-Ru三元复合催化剂的二氯喹啉酸绿色合成工艺。以3,7-二氯-8-二氯甲基喹啉(M2)作原料,双氧水作氧化剂,通过优化催化剂组成、反应温度等控制条件,显著提高了反应效率和环境友好性。实验结果表明:催化剂总量为底物M2质量的8%,在Cu(OAc)_(2)∶Co(OAc)_(2)∶RuCl_(3)(质量比)=3∶3∶2、90~100℃条件下,二氯喹啉酸质量分数可达95.2%,收率达93.6%。新工艺消除了硝酸/硫酸的使用,避免了高温高压操作,为工业化生产提供了安全经济的技术方案。 展开更多
关键词 二氯喹啉酸 复合催化剂 绿色合成 氧化 3 7-二氯-8-二氯甲基喹啉
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使用1,2,3,4-四氯丁烷制备2,3-二氯-1,3-丁二烯
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作者 李德胜 杨振林 +1 位作者 王美 高兴博 《山东化工》 2025年第1期31-33,38,共4页
通过使用1,2,3,4-四氯丁烷为主要原料,以氢氧化钠作为脱除剂,以氧化胺作为相转移催化剂,以吩噻嗪作为阻聚剂,在一定温度下反应,再通过减压蒸馏得到较高纯度的2,3-二氯-1,3-丁二烯。实验中分别采用水、乙醇、甲醇作为脱除剂溶剂,并调整... 通过使用1,2,3,4-四氯丁烷为主要原料,以氢氧化钠作为脱除剂,以氧化胺作为相转移催化剂,以吩噻嗪作为阻聚剂,在一定温度下反应,再通过减压蒸馏得到较高纯度的2,3-二氯-1,3-丁二烯。实验中分别采用水、乙醇、甲醇作为脱除剂溶剂,并调整脱除剂中氢氧化钠质量分数、反应温度及保温时间,探究合成2,3-二氯-1,3-丁二烯最佳工艺方法。实验结果表明,使用氢氧化钠甲醇溶液作为脱除剂溶液,其中氢氧化钠质量分数为20%,反应温度为60℃,反应时间为50~70 min时,可以得到高纯度、高收率的2,3-二氯-1,3-丁二烯。 展开更多
关键词 2 3-二氯-1 3-丁二烯 消去反应 相转移催化剂
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N-[反式-2-(3,4-~3H-吡咯基)-环己基]-N-甲基-3,4-二氯-苯乙酰胺盐酸盐的合成
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作者 李德有 马斯才 +2 位作者 李健国 王崇铨 沈德存 《中国药物化学杂志》 CAS CSCD 1990年第1期66-68,共3页
N-[反式-2-(1-吡咯基)环己基]-N-甲基-3,4-二氯-苯乙酰胺盐酸盐(简称U-50488H(K-I))是近年来报道的高选择性的K-阿片受体激动剂,动物实验结果表明:该化合物具有较强的镇痛活性,且成瘾性较低,呼吸抑制较弱,无吗啡样副作用的新型麻醉镇痛... N-[反式-2-(1-吡咯基)环己基]-N-甲基-3,4-二氯-苯乙酰胺盐酸盐(简称U-50488H(K-I))是近年来报道的高选择性的K-阿片受体激动剂,动物实验结果表明:该化合物具有较强的镇痛活性,且成瘾性较低,呼吸抑制较弱,无吗啡样副作用的新型麻醉镇痛剂。为研究它的药理作用,我们用氚标记了U-50488(K-I)。合成该化合物开始原料是N-甲基-反式-2-(1-△~3-吡咯啉基)环己基胺,按一般还原法以氧化铂为催化剂,通氚进行氚化反应,未经分离与3,4一二氯苯乙酸在二环己基碳二亚胺(DCC)存在下进行缩合脱水反应,生成N-[反式-2-(3,4-~3H-吡咯基)环己基]-N-甲基-3,4-二氯-苯乙酰胺,再用氯化氢乙醚处理,制得了氚化的U-50488(K-I)。合成途径如下: 展开更多
关键词 ANALGESIC activity N-[trans-2-(3 4-~3H-pyrrolyl)-cyclohexyl)-N-methyl-3 4-dichloro-benzenacetamide hydrochloride
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A 24-metal Cd_((II))-Sm_((III))nanocage with a rapid triple-emissive response for 2,6-dichloro-4-nitroaniline
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作者 Yuebo Cheng Yanan Ma +3 位作者 Xiaoping Yang Hao Li Zhen Zhang Desmond Schipperd 《Inorganic Chemistry Frontiers》 2023年第2期417-423,共7页
A 24-metal Cd_((II))-Sm_((III))nanocluster[Cd_(18)Sm_(6)L_(9)(OAc)_(3)_(6)](CSN)was constructed from a new flexible Schiff base ligand.It can be used as a probe to detect 2,6-dichloro-4-nitroaniline(DCN,LOD:0.67-0.75... A 24-metal Cd_((II))-Sm_((III))nanocluster[Cd_(18)Sm_(6)L_(9)(OAc)_(3)_(6)](CSN)was constructed from a new flexible Schiff base ligand.It can be used as a probe to detect 2,6-dichloro-4-nitroaniline(DCN,LOD:0.67-0.75μM),which is not influenced by the presence of other pesticides.The response behavior of CSN to DCN is expressed using a first-order equation 1/I_(475nm)+1/I_(645nm)+1/I_(945nm)=A[DCN]+B,and it is used to determine DCN concentrations in the extract of fruits.For example,for the concentration determination of DCN in carrot extract,the ranges of recovery and RSD are 96.11-103.50%and 0.95-4.12%,respectively. 展开更多
关键词 detection dichloro nitroaniline triple emissive response cd ii sm iii nanocage determine dcn recovery probe flexible schiff base ligandit
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Preparation and Purification of Halogenated Hydroxydiphenyl Ethers 被引量:1
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作者 宋健 冯荣秀 +3 位作者 陈磊 王军波 石巍 王琨 《Transactions of Tianjin University》 EI CAS 2002年第1期37-39,共3页
As a good antimicrobial active ingredient, 2,4,4′ trichloro 2′ hydroxydiphenyl ether has been already commercially available since 1970s. For this paper halogenated hydroxydiphenyl ethers were prepared and purifi... As a good antimicrobial active ingredient, 2,4,4′ trichloro 2′ hydroxydiphenyl ether has been already commercially available since 1970s. For this paper halogenated hydroxydiphenyl ethers were prepared and purified, and their analytical conditions by HPLC were studied. Further purification of 2,4,4′ trichloro 2′ hydroxydiphenyl ether was also studied. The adsorption ability of different decolourants, e.g. alumina and bentonite, for each component in crude product of 2,4,4′ trichloro 2′ hydroxydiphenyl ether was varied. 2,4,4′ trichloro 2′ hydroxydiphenyl ether might be adsorbed by active carbon. The colored impurities might be adsorbed by alumina. The colorless impurities might be adsorbed by bentonite. 展开更多
关键词 trichloro 2′ hydroxydiphenyl ether 2 6 4′ trichloro 2′ hydroxydiphenyl ether 4 4′ dichloro 2′ hydroxydiphenyl ether PURIFICATION
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