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以二苯胺和乙二酰氯为起始原料经偶联、酰化、还原反应得到1-苯基吲哚,并探索了其影响因素。结果表明合成中间体N,N-二苯基-2-氯-2-氧代乙酰胺的较佳条件为:n(二苯胺):n(乙二酰氯)=1∶3,反应温度20~25 ℃,反应2.5 h,收率98.02%,HPLC纯度97.68%;产品1-苯基靛红的较优合成工艺条件为: n(N,N-二苯
基-2-氯-2-氧代乙酰胺) :n(无水AlCl3)=1∶3,反应温度10 ℃,反应时间2 h,收率86.76%,HPLC纯度98.45%;目标产物1-苯基吲哚的最佳工艺条件为:n(1-苯基靛红):n(硼氢化钠)=1∶3,n(1-苯基靛红):n(氯化锌)=1∶0.05,反应温度110 ℃,反应时间12 h,收率72.41%,HPLC纯度98.14%。产品及中间体结构经1H NMR、MS和显微熔点仪分析表征确认。 相似文献
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以吗啉和一氯化硫为原料,以固体氢氧化钠为缚酸剂合成了N,N’-二硫代二吗啉(DTDM),考察了反应条件和重结晶条件对产物收率的影响。结果表明,较佳的合成工艺条件为:n(吗啉)∶n(S2Cl2)∶n(NaOH)=2∶1∶2,反应温度30~40℃,反应时间8 h,粗产品收率可达93%;较佳的重结晶工艺条件为:溶剂乙酸乙酯,m(溶剂)∶m(产品)=4∶1,结晶温度0~5℃,重结晶收率可达93%,DTDM总收率可达86%以上,采用FTIR与1H NMR对产物结构进行了表征。 相似文献
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由乙二胺和对甲苯磺酰氯反应制得N,N′-双(对甲苯磺酰基)乙二胺。此步最佳工艺条件为:n(对甲苯磺酰氯)∶n(乙二胺)=2.2∶1,反应溶剂为苯,反应温度为40~45℃,反应时间为6h,收率80%。由丙烯酸甲酯和溴反应制得α,β-二溴丙酸甲酯,收率为88%。再由上述二种中间体反应合成标题化合物,此步省略了N,N′-双(对甲苯磺酰基)乙二胺的二钠盐制备,收率为73%。 相似文献
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N,N’-双月桂酰基乙二胺二乙酸钠合成方法的改进 总被引:1,自引:0,他引:1
对表面活性剂N,N’-双月桂酰基乙二胺二乙酸钠的合成方法进行了改进。以月桂酸、乙二胺和氯乙酸为原料制得N,N’-双月桂酰基乙二胺二乙酸钠。考察了反应温度、反应时间、原料配比对中间体合成的影响。结果表明,N,N’-双月桂酰基乙二胺(中间体Ⅰ)的最佳合成条件是:n(月桂酰氯)∶n(乙二胺)=3.5∶1,反应温度70℃,反应时间1 h,产率为96.94%;N,N’-双月桂酰基乙二胺二乙酸(中间体Ⅱ)的最佳合成条件是:n(氯乙酸)∶n(中间体Ⅰ)=3∶1,反应温度65℃,反应时间12 h,产物产率为53.38%。产物结构用红外光谱、元素分析等方法进行了表征。 相似文献
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N,N-二乙基氨基乙基-3,4-二氯苄基醚及其类似物的合成 总被引:1,自引:0,他引:1
用相转移催化法合成了5个N,N-二乙基氨基乙基-3,4-二氯苄基醚及其类似物,产率为72%~86%。适宜的反应条件是:以二烷基氨基乙醇、3,4-二氯氯化苄为原料,在固体氢氧化钠作用下,四丁基溴化铵为相转移催化剂,甲苯为溶剂,n(R1R2NCH2CH2OH)∶n(C l2ArCH2C l)∶n(NaOH)∶n(PTC)=1.1∶1∶2∶0.05,反应时间2 h,温度70℃。产物经沸点、元素分析、红外光谱、核磁共振氢谱予以确证。 相似文献
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以N,N-二甲基苯胺为原料,经与PCl_3和吡啶反应生成[(4-(N,N-二甲氨基)苯基)二氯化磷(Ⅰ),然后在CuI和LiBr的催化作用下与叔丁基氯化镁反应制得[(4-(N,N-二甲氨基)苯基)二叔丁基磷(Ⅱ)。产物的结构经~(31)PNMR、~1HNMR和HRMS表征。通过考察各步反应条件,得出最佳工艺条件为:n(N,N-二甲基苯胺)∶n(PCl_3)∶n(吡啶)=1∶3∶3,110℃反应24 h,Ⅰ的收率为85.3%;n(Ⅰ)∶n(CuI)∶n(LiBr)∶n(叔丁基氯化镁)=1∶0.1∶0.2∶3,40℃反应12 h,Ⅱ的收率为83.4%。 相似文献
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以氯乙酸甲酯、4-苯氧基苯酚为原料,在无水碳酸钾存在下,N,N-二甲基甲酰胺(DMF)为溶剂,制备了中间体2-(4-苯氧基苯氧基)乙酸甲酯(Ⅰ),进而,中间体(Ⅰ)和二甲胺反应。得到目的产物N,N-二甲基-2-(4-苯氧基苯氧基)乙酰胺(Ⅱ)。考察了反应温度、反应时间、物料投料比对目的产物(Ⅱ)收率的影响,从而确定了合成工艺条件为:反应温度15~20°C;反应时间3.5~4 h;物料投料比n(Ⅰ)∶n(二甲胺)=1.0∶1.4。在此条件下,N,N-二甲基-2-(4-苯氧基苯氧基)乙酰胺的收率达80%以上。化合物的结构经IR1、H NMR和元素分析进行了表征。 相似文献
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以自制的中间体N,N-二(2-羟乙基)-2-氨基丙烯为原料,对其进行磺化反应,控制温度、时间和摩尔比反应合成磺酸型水性聚氨酯扩链剂N,N-二(2-羟乙基)-2-氨基丙磺酸钠,借助核磁氢谱(1H NMR)、红外光谱(FTIR)、元素分析、X射线衍射(XRD)等手段对合成产物进行了组成、结构和结晶性表征,用热重分析仪表征了产物的热稳定性。根据产物的磺化度确定最佳的合成工艺:反应温度为90℃,反应时间为8 h,N,N-二(2-羟乙基)-2-氨基丙烯和亚硫酸氢钠(NaHSO3)的物料比为1:2.5,磺化率可达到94%以上。分别以二羟甲基丙酸(DMPA)和自制磺酸型单体作为亲水扩链剂制备羧酸型水性聚氨酯(CWPU)和磺酸型水性聚氨酯(SWPU),其性能对比结果表明:SWPU相比于CWPU具有较好的亲水性和耐热性能;固含量及稳定性方面,SWPU也是优于CWPU的。 相似文献
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反应挤出法制备POE-g-(GMA-co-St)的研究 总被引:1,自引:0,他引:1
以甲基丙烯酸缩水甘油酯(GMA)为接枝单体,苯乙烯(St)为接枝共单体,在双螺杆挤出机上对乙烯-辛烯共聚物(POE)进行熔融接枝,制备了POE—g-(GMA—co—St)。研究了引发剂用量、单体用量、共单体用量和抑交联剂亚磷酸三苯酯等对POE接枝物接枝率和熔体流动速率的影响,利用红外光谱对接枝物进行了表征。研究袭明,St的加入能有效提高GMA的接枝率,亚磷酸三苯酯有效抑制了POE的交联。最佳配方为:过氧化二异丙苯(DCP)为0.15份,GMA为3份,St为3份,亚磷酸三苯酯为1份。 相似文献
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A dicarboxylic acid ( 1 ) bearing two phthalimide rings was prepared by the condensation of N-phenyl-3,3-bis[4-(4-aminophenoxy)phenyl]phthalimidine and trimellitic anhydride. A new family of poly(amide–imide)s having inherent viscosities of 0.65–1.65 dl/g was prepared by the triphenyl phosphite activated polycondensation of the diimide–diacid 1 with various aromatic diamines in a medium consisting of N-methyl-2-pyrrolidone (NMP), pyridine, and calcium chloride. All the resulting polymers showed an amorphous nature and were readily soluble in polar solvents such as NMP and N,N-dimethylacetamide. The soluble poly(amide–imide)s afforded transparent, flexible, and tough films. The glass transition temperatures of these polymers were in the range 249–340°C and the 10% weight loss temperatures were above 545°C in nitrogen. 相似文献
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Jinghui Yang Zhanhai Yao Dean Shi Hongliang Huang Yong Wang Jinghua Yin 《应用聚合物科学杂志》2001,79(3):535-543
Grafting of acrylic acid and glycidyl methacrylate onto low density polyethylene (LDPE) was performed by using a corotating twin‐screw extruder. The effects of residence time and concentration of initiator and monomers on degree of grafting and gel content of grafting LDPE were studied systematically. Paraffin, styrene, p‐benzoquinone, triphenyl phosphite, tetrachloromethane, and oleic acid were added to try to decrease the extent of crosslinking of LDPE. 4‐hydroxyl‐2,2,6,6‐tetramethyl‐1‐piperidinyloxy (4‐hydroxyl‐TEMPO) and dipentamethylenethiuram tetrasulfide were also tried to inhibit crosslinking reaction of LDPE during its extruding grafting process. It was found that p‐benzoquinone, triphenyl phosphite and tetrachloromethane were good inhibitors for crosslinking of LDPE. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 79: 535–543, 2001 相似文献
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Shadpour Mallakpour Mohammad Dinari Shekoofeh Neamani 《Polymer-Plastics Technology and Engineering》2015,54(15):1634-1643
This study aimed at preparing three nanocomposites of optically active poly(amide–imide) and zirconium dioxide (ZrO2) inorganic nanoparticles through the ultrasonic process. First, the surface of ZrO2 nanocomposites was chemically modified with bio-active citric acid in the basic media. Then, the poly(amide–imide) was reinforced with modified nanocomposites and three poly(amide–imide)/ZrO2-citric acid nanocomposites were synthesized by ultrasonic irradiation. The poly(amide–imide) was prepared by polycondensation of N-trimellitylimido-L-leucine with 4,4′-diaminodiphenylsulfone using of triphenyl phosphite and molten tetra-n-butylammonium bromide as green media. The obtained poly(amide–imide)/ZrO2-citric acid nanocomposites were characterized by different techniques. 相似文献
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《Carbon》2013
Eight organophosphorus compounds, trimethyl phosphate (TMP), tributyl phosphate (TBP), triphenyl phosphate (TPP), trimethyl phosphite (TMPI), tributyl phosphite (TBPI), triphenyl phosphite (TPPI), diethyl phosphite (DEPI) and diphenyl phosphoryl chloride (DPPC), were employed as activating agents to prepare activated carbons (AC-OPCs) from lotus stalks (LS). AC-OPCs contained mostly micropores with only a small contribution of mesopores and their pore sizes were mainly below 4 nm. Physical and chemical analysis results indicated that activations with OPCs dramatically enhanced the porosity, yield and surface acidity of AC-OPCs. 相似文献