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在DMF溶剂中,不外加催化剂使邻取代芳香醛(1)与5,5-二甲基-1,3-环己三酮(2)发生缩合和加成反应生成3,3,6,6-四甲基-4a-羟基-9-芳基-1,8二氧化-2,3,4,4a,5,6,7,8,9a-十氢化-1H氧杂蒽(3a~3d)。在同样条件下,邻羟基芳香醛与5,5-二甲基-1,3-环己三酮则发生缩合,加成和脱水反应生成3,3-二甲基-9-(5,5-二甲基-3-羟基-2-环己烯-1-酮-2-基)-1-氧代-2,3,4,9-四氢化-1 氧杂蒽(4a~4b)。用单晶X-射线分析法确定了产物3a和4a的晶体结构。 相似文献
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蒽酮1和氯甲基吡啶盐酸盐2在甲苯中回流反应生成10,10-二吡啶甲基-9(10H)蒽酮(3),收率63%~68%;3用硼氢化钠还原生成10,10-二吡啶甲基-9,l0-二氢蒽-9-醇(4),收率87%~90%;蒽醇4在酸催化下发生歧化反应,得到还原产物10,10-二吡啶甲基-9,10-二氢蒽(5)和氧化产物蒽酮3.该歧化反应受催化剂、溶剂和反应温度等影响.当蒽醇4用三氟化硼为催化剂、甲苯为溶剂、回流反应,5的收率达到74%.所合成的新化合物都经1H NMR,13C NMR,MS和元素分析表征确认. 相似文献
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2-氰基-2,3-二甲基-3-甲基羰甲基-5-硫酮-吡咯烷的合成 总被引:2,自引:0,他引:2
2-氰基-2;3-二甲基-3-甲基羰甲基-5-硫酮-吡咯烷的合成;双甲基环并内酯;双甲基环并内酰胺-内酯;氰基吡咯烷酮;氰基吡咯烷硫酮 相似文献
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以环己烯酮和硝基乙酸乙酯为原料,经Michael加成、水解脱羧、亲核氟化和还原反应合成了3,3-二氟环己基甲胺(4),总收率55%,其结构经1H NMR和MS确证。在最佳还原反应条件[1,1-二氟-3-硝甲基环己烷83.73 mmol, Raney Ni (80%)和NH3·H2O为共催化剂,EtOH为溶剂,于室温反应12 h]下,4的收率82%。 相似文献
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本文以4-甲基邻苯二甲酸酐为原料, 成功地合成了5,5′-二甲基-2,2′-二茚满-1,1′,3,3′-四酮(2). 通过元素分析、核磁共振、红外光谱及质谱等测试手段, 确定了化合物2的结构与存在形式, 通过ESR测试发现化合物2具有顺磁性. 相似文献
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A New Capillary Electrophoresis Apparatus with Piezoelectric Ceramics High Voltage Source and Amperometric Detector 总被引:13,自引:0,他引:13
Zuan Guang CHENI Jin Yuan MO Xiao Yun YANG Li Shi WANG Xue Ting MEIZ Min Sheng ZHANGI 《中国化学快报》1999,(3)
IntroductionHighperformancecapiliar}'electrophoresis(HPCE)isanewanalyticaltechnology'rapidly'developedinrecentyears.Withtheadvantagesofsmallsample.highsensitivity,highresolution.rapidanalysisandverycheaprunning,ithasbeenappliedinchemistry'.lifescienc... 相似文献
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Dawson型磷钨酸催化合成乳酸月桂醇酯 总被引:1,自引:0,他引:1
用Dawson型磷钨酸催化合成乳酸月桂醇酯。实验结果表明:Dawson型磷钨酸有较高的催化活性,反应时间短,酯收率高,工艺简单。最佳工艺条件为:醇/酸摩尔比为1.5:1,催化剂用量为0.3%,带水剂甲苯体积(mL)与反应物质量(g)之比为0.4:1~0.5:1,反应温度为115~140℃,反应时间30~50min。在此条件下,酯收率可超过93% 。 相似文献
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以松香,环氧氯丙烷,甲醛及苯酚等为主要原料,合成了一种新型的环氧树脂。通过正交实验法确定了环氧化反应的最佳实验条件,即环氧化温度90℃,碱用量13 g,催化剂为cat 1,其最佳用量为0.018 mol,环氧氯丙烷的用量为50 g,碱浓度为30%(以上数值均以松香用量为70 g时计)。在最佳实验条件下合成得到了松香改性酚醛环氧树脂(简称RAPE),并用HPLC、FT-IR、NMR对其进行结构表征。结果表明,得到的RAPE其环氧值为0.28 mol/100g,平均聚合度约为3.4,酚羟基和树脂酸上的羧基基本反应完全,得到一种新型的缩水甘油醚型和缩水甘油酯型的环氧树脂。 相似文献
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An application of polyacrylamide-grafted-gum ghatti (PAAm-g-GGH) copolymer for transdermal delivery of an anti-psychotic drug, quetiapine fumerate triggered by electric stimulus was explored. The electro-responsive PAAm-g-GGH was prepared by free radical polymerization underneath nitrogen atmosphere subsequent to alkaline hydrolysis. The PAAm-g-GGH was used as drug reservoir gel and crosslinked films of GGH and PVA as rate controlling membranes (RCM). The reservoir gels were uniform and translucent; pH of gels was 6.56–7.06, which is in the pH range of skin and drug content was from 89.57% to 94.51%. The thickness of RCMs was 163–227?μ; thickness was increased with increased glutaraldehyde concentration and all the RCMs were permeable to water vapors. When electric stimulus was absent, a small amount of drug was permeated from the formulations, while drug conveyance was enhanced in the existence of stimulus. Drug permeation was increased with increase in electric stimulus from 2 to 8?mA. Over two fold increase in flux was observed after application of electric stimulus. Under “on–off” electric stimulus, faster drug permeation was seen under ‘on’ condition and permeation was decreased when stimulus was ‘off.’ Histopathology study confirmed reversible alteration of skin structure under electric stimulus. 相似文献
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Selective flow-injection determination of methanol in the presence of ethanol based on a multi-enzyme system with chemiluminescence detection 总被引:2,自引:0,他引:2
Yoshiie Sekine
Masayasu Suzuki
Toshifumi Takeuchi Eiichi Tamiya Isao Karube 《Analytica chimica acta》1993,280(2):179-184A highly selective flow-injection system was developed for the determination of methanol. The system consisted of three immobilized enzymes with luminol chemiluminescence detection. First, methanol was oxidized in the presence of alcohol oxidase to yield formaldehyde and hydrogen peroxide. The hydrogen peroxide produced was then destroyed by catalase. The formaldehyde formed in the first stage was further oxidized by NAD+-formaldehyde dehydrogenase. The NADH formed was oxidized by 1-methoxy-5-methylphenazinium methylsulphate (1-MPMS), and finally the reduced 1-MPMS was spontaneously oxidized and hydrogen peroxide was produced. The concentration of the hydrogen peroxide produced, which was proportional to the initial concentration of methanol, was determined by luminol chemiluminescence. The determination range was from 0.1 to 100 mg l−1 and the response time was less than 2 min per sample with a relative standard deviation of less than 3%. The system showed good selectivity for methanol; the response was ca. 50 times higher than for ethanol. 相似文献
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植物油酸新戊二醇对苯二甲酸复合酯的合成及性能 总被引:1,自引:0,他引:1
用新戊二醇(NPG)和对苯二甲酰氯(TPA)反应生成“低聚物”中间体,当n(NPG)/n(TPA)由2.4增加至3.0时,中间体的聚合度(m)在3.5~1.45之间,收率75.5%。再将中间体与油酸、菜籽油酸进行酯化得到复合酯,收率88.5%。结果表明,复合酯的粘度随着分子量的增大而增大,粘度指数大于125,凝点低于-27℃,氧化稳定性随分子量的增大而提高,生物降解率>70%,最大无卡咬负荷(PB)为784N,磨斑直径0.41mm,热分解温度>250 ℃,因此植物油酸新戊二醇对苯二甲酸复合酯是性能良好的绿色润滑剂。 相似文献
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海藻酸钠-壳聚糖微胶囊膜强度的研究 总被引:23,自引:0,他引:23
以乳化/内部凝胶化法制备了海藻酸钠-壳聚糖微胶囊,重点考察了成膜反应过程中影响微胶囊膜强度的几个主要参数,实验发现,壳聚糖分子量低于100000,成膜反应时间高于15min,壳聚糖溶液pH值在6.0左右时制备的微胶囊膜强度较高.初步探讨了海藻酸钠与壳聚糖两种高分子发生聚电解质络合反应的机制. 相似文献