N—甲基哌嗪的合成研究

介绍了Ｎ－甲基哌嗪的物化性质，综述了以乙醇胺、哌嗪等不同结构物质为原料合成了２－甲基哌嗪的几种方法。     

不饱和醇型檀香的合成与分析

在合成檀香化合物３－甲基－５－（２，２，３－三甲基环戊－３－烯－１－基）－戊－２－醇的过程中，对前体化合物３－甲基－５－（２，２，３－三甲基环戊－３－烯－１－基）－３－烯－２－酮采用化学还原方法，合成出不饱和醇型檀香化合物３－甲基－５－（２，２，３－三甲基环戊－３－烯－１－基）－３－烯－戊－２－醇，对其进行了物理常数、ＩＲ、￣１ＨＮＭＲ、ＧＣ－ＭＳ的分析测定。     

2—甲基哌嗪的合成

介绍以环氧丙烷为原料，用两步法制备２－甲基哌嗪，总收率６０．２％。     

含2－哌嗪酮缓蚀剂的水性脱酯清洗剂配方

９４－０１４含２－哌嗪酮缓蚀剂的水性脱酯清洗剂配方化合物４－（２－羟乙基）－２－嗪酮或Ｎ，Ｎ’－二甲基－２－嗪酮用于含有阴离子和非离子表面活性剂的水性清洗剂中，以抑制冷轧钢清洗脱酯时表面腐蚀。含2－哌嗪酮缓蚀剂的水性脱酯清洗剂配方...     

2—甲基哌嗪合成方法的改进

２┐甲基哌嗪合成方法的改进徐建伟（同济大学测试中心，上海２０００９２）魏宏斌＊（同济大学环境工程学院，上海２０００９２）２－甲基哌嗪（Ⅰ）是喹诺酮类抗生素、抗过敏和抗肿瘤药物的一种重要中间体，有关它的合成方法已有报道［１～４］。但是收率较好的合成方法...     

2—甲基—3（4）—乙酰硫基呋喃的合成

以２－甲基呋喃为原料合成了含硫香料化合物２－甲基－３（４）－乙酰硫基呋喃，并对其结构进行了分析鉴定。     

2－甲基－3（4）－乙酰硫基呋喃的合成

以２－甲基呋喃为原料合成了含硫香料化合物２－甲基－３（４）－乙酰硫基呋喃，并对其结构进行了分析鉴定。     

2—甲基—3（4）—呋喃硫醇的合成

从２－甲基－３（４）－乙酰硫基呋喃合成了香料化合物２－甲基－３（４）－呋喃硫醇，并对产品进行了分析鉴定。     

2－甲基－3（4）－异丁硫基呋喃的合成

以２－甲基呋喃为原料合成肉味香料化合物２－甲基－３（４）－异丁硫基呋喃，对其结构进行了分析和鉴定。     

涂料防霉剂N—（4—溴—2—甲基苯基）氯乙酰胺的合成

由２－甲基苯胺出发，经Ｎ－（２－甲基苯基）乙酰胺的选择性单溴化，再水解成４－溴－２－甲基苯胺，后者与氯乙酰氯反应，制得了标题化合物。     

Electrophoretic deposition of polyetherimide from an aqueous emulsion: optimisation of some deposition parameters

A systematic study was carried out to investigate the cataphoretic electrodeposition of polyetherimide from an aqueous medium onto an electrically conductive support (aluminum, steel mesh). The subsequent re‐imidisation steps were also investigated. The yield and quality of deposited polyetherimide were found to be strongly dependent upon a number of formulation variables that are closely related to the emulsion composition and electrodeposition conditions. A polymer modified to 70% with methylpiperazine and quaternised to 50% with lactic acid gave a stable emulsion at 6% w/w (seven days at 4–5 °C). Maximum rate of deposition was obtained with an initial current density of 10 mA cm⁻² in the voltage range of 40–68 V. © 1999 Society of Chemical Industry     

Novel Imatinib Derivatives with Altered Specificity between Bcr–Abl and FMS,KIT, and PDGF Receptors

Imatinib is a clinically important ATP analogue inhibitor that targets the tyrosine kinase domain of the intracellular Abl kinase and the PDGF receptor family. Imatinib has revolutionised the treatment of chronic myeloid leukaemia, which is caused by the oncogene Bcr–Abl and certain solid tumours that harbor oncogenic mutations of the PDGF receptor family. As a leading kinase inhibitor, imatinib also provides an excellent model system to investigate how changes in drug design impact biological activity, which is an important consideration for rational drug design. Herein we report a new series of imatinib derivatives that in general have greater activity against the family of PDGF receptors and poorer activity against Abl, as a result of modifications of the phenyl and N‐methylpiperazine rings. These new compounds provide a platform for further drug development against the therapeutically important PDGF receptor family and they also provide insight into the engineering of drugs with altered biological activity.     

N─甲基哌嗪-哌嗪及水-N─甲基哌嗪二元体系汽液平衡的研究

The VLE data for binary systems of N-methylpiperazine-piperazine and water-N- methylpiperazine were measured at pressure of 0.1013 MPa by using an improved Rose still.The experimental data of the systems were tested for thermodynamic consistency and correlated satisfactorily with Wilson equation.The critical properties,pc,Tc,V_c,and acentric factors,ω,of both N-methylpiperazine and piperazine have been estimated by group contribution method.The UNIFAC model was successfully used to correlate and predict VLE data of N-methylpiperazine-piperazine system．     

左氧氟沙星合成工艺改进研究

对左氧氟沙星的工艺进行了优化,以(2,3,4,5)-四氟苯甲酰氯为起始原料,经酰化,胺化,环合制得左氧氟环合酯,然后用无水哌嗪与左氧氟环合酯缩合,经硫酸二甲酯甲基化后水解精制得左氧氟沙星。与原工艺相比,用无水哌嗪代替N-甲基哌嗪,提高了产品的收率和质量,降低了成本,减少了环境污染,技术指标符合CP2010左氧氟沙星要求。     

Ultrafiltration of metal ions by water‐soluble chelating poly(N‐acryloyl‐N‐methylpiperazine‐co‐N‐acetyl‐α‐aminoacrylic acid)

Water‐soluble copolymers of N‐acryloyl‐N‐methylpiperazine and N‐acetyl‐α‐aminoacrylic acid were synthesized by radical polymerization. The copolymerization yield ranged between 60 and 97%. The FTIR and NMR spectra demonstrated that the copolymerization occurred. The copolymer composition was determined from ¹H‐NMR spectra by comparison of methyl groups from both moieties. The copolymers were richest in AAA units. The metal ion retention properties were investigated by the liquid‐phase polymer‐based retention (LPR) technique at different pH and filtration factors. The affinity for the metal ions depended on the copolymer composition, pH, and filtration factor. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 2556–2561, 2002     

Water‐sorption and metal‐uptake behavior of pH‐responsive poly (N‐acryloyl‐N′‐methylpiperazine) gels

Hydrogels based on N‐acryloyl‐N′‐methylpiperazine (AcrNMP) swelled extensively in solutions of low pH due to the protonation of the tertiary amine. The water transport in the gels under an acidic condition was non‐Fickian and nearly Fickian in neutral pH with the collective diffusion coefficients determined as 2.08 × 10⁻⁷ and 5.00 × 10⁻⁷ cm⁻² s⁻¹, respectively. These gels demonstrated good metal‐uptake behavior with various divalent metal ions, in particular, copper and nickel, with the uptake capacity increased with increasing pH. The swelling ratio of the gel in the presence of metal ions decreased with increasing metal ion uptake. The results suggest that high metal ion uptake can lead to physical crosslinking arising from the interchain metal complex formation. The metal‐loaded gels could be stripped easily with 1M H₂SO₄ without any loss in their uptake capacity. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 268–273, 2001     

Efficient and Selective Synthesis of E‐Vinylamines via Tungsten(0)‐Catalyzed Hydroamination of Terminal Alkynes

The hydroamination of terminal alkynes (RCCH=phenylacetylene, 4‐methylphenylacetylene, 4‐fluorophenylacetylene, 1‐hexyne, methyl 2‐propynyl ether, prop‐2‐yn‐1‐ol) with secondary amines (piperidine, pyrrolidine, morpholine, piperazine, methylpiperazine, 4‐methylpiperidine and 3‐methylpiperidine) was achieved in high yield (up to 99%), regioselectivity (only anti‐Markovnikov product) and stereoselectivity (only E‐isomers) within a maximum of 5 h in reactions catalyzed by the tungsten tetracarbonyl complex cis‐[W(CO)₄(piperidine)₂] at 90 °C without any additional solvent.

     

SPME-GC-MS分析榴莲果肉中的挥发性成分

为了研究榴莲果肉中的挥发性香气成分,采用两种固相微萃取纤维提取了榴莲果肉中的挥发性成分,并利用气相色谱-质谱联用技术对所得挥发性成分进行了分离与鉴定。采用保留指数和质谱进行定性,共鉴定出60种挥发性成分,其中酯类26种,含硫化合物12种,醇类7种,烃类7种,醛类3种,酸类2种、含氮化合物2种和酚类1种;采用面积归一化法确定了它们相对含量,相对含量较高的是2-甲基丁酸乙酯、丙酸乙酯、1-十四醇、乙酸乙酯、丁酸乙酯、反-2-丁烯酸乙酯、二乙基二硫醚、2-甲基丁酸丙酯、十四醛、乙硫醇。从鉴定出的挥发性成分的香气特征可知,榴莲的香气主要是由酯类化合物和含硫化合物赋予的,其中大多数酯类化合物是脂肪酸乙酯,含硫化合物中硫醇和硫醚的含量相对较高。     

过渡金属-取代钨硅杂多阴离子层状材料催化剂催化乙酸正丁酯的合成

用离子交换法将具有Keggin结构的K8[SiW11MO40]（M=Co^2＋，Cu^2＋，Ni^2＋）嵌入到Zn2Al黏土中，得到层状化合物Zn2Al-SiW11M（M=Co^2＋，Cu^2＋,Ni^2＋），并用XRD，IR，UV对其进行了表征。结果表明：杂多阴离子进入黏土后，仍保留了其Keggin结构。利用层状化合物催化合成乙酸正丁酯，考察其催化活性。结果表明：层状化合物在酯化反应中显示出优良的催化性能。     

水杨醛型Schiff碱配合物的合成、表征与磁性研究

以乙醇为溶剂、水杨醛缩邻氨基苯酚(L)与过渡金属(M)硝酸盐或醋酸盐作用,制得了6个LM及6个L2M配合物(合成过程中须将反应混合液蒸馏至干才能得到Cr、Fe、Ni的配合物)。对所制备的配合物进行了摩尔电导、磁化率、DTA、SEM、UV、IR等表征。结果表明:LM(M=Cr3+、Mn2+、Fe3+、Co2+)为平面正方形场低自旋型;LNi、LCu及L2M(M=Mn2+,Co2+,Cu2+)为四面体场高自旋型;其余经蒸馏得到的L2M(M=Cr3+,Fe3+,Ni2+)则为八面体场配合物。配合物均为顺磁性,除LCr、LFe、LCu及L2Cu也有电子轨道运动的贡献外,磁性主要是电子自旋运动的贡献,LM分子中有水参与配位,并有分子内氢键形成。