氧芐羟胺盐酸盐的简便合成

氧芐基羟胺盐酸盐可通过苯甲羟肟酸的氧苄醚化、酸水解及氯化氢成盐制得,总收率76%。     

植物生长调节剂羧甲基羟胺半盐酸盐的合成

介绍了羟胺盐酸盐和氯乙酸为主要原料合成羧甲基羟胺半盐酸盐工艺,羧甲基羟胺半盐酸盐是应用于切花保鲜的植物生长调节剂,该工艺具有工业化可行性。     

氧取代羟胺盐的合成研究进展

综述了氧取代羟胺盐的几种合成方法,并对其前景做了展望.     

电化学还原硝基甲烷合成N-甲基羟胺盐酸盐的工业化试验

An industrial electrolytic cell was designed for the electrochemical synthesis of N-methylhydroxylamine hydrochloride （N-MHA）. Copper was used as the cathode, graphite as the anode, and a cation membrane as the separator. The results show that N-MHA with a high purity of 99% can be electrosynthesized directly from nitromethane in HC1 solution. Under a constant current of 1000-2500A.m^-2 in the temperature of 30-50℃, the average yield, current efficiency, and reaction selectivity were 65%, 70%, and 99%, respectively. Graphite electrode and membrane material can be used continuously in the preparative electrolysis for 5000h. Moreover, the effects of the electrode and membrane materials, current intensity, electrolyte temperature, and other associated parameters on the electrosynthesis results were investigated. The direct current power consumption was 8151.3kW-h-（1000kg N-MHA）^ -1. This method is a simple separation process with limited contamination and hence, is a new green synthesis method for the industrial production of N-MHA.     

O-邻氟苯甲基羟胺盐酸盐的合成

以丙酮肟和邻氟氯苄为原料合成了O-2-氟苯甲基丙酮肟醚,再用盐酸水解得到了O-2-氟苯甲基羟胺盐酸盐。文章系统研究了反应温度、不同溶剂、溶剂含水量等各种实验因素对O-2-氟苯甲基丙酮肟醚的影响,研究了盐酸浓度、水解温度等因素对O-2-氟苯甲基丙酮肟醚水解工艺的影响。两步收率最高分别为92.3%和87.3%。并用核磁等对产品及中间体进行了表征。     

N-苄氧羰基氨基酸的合成

以甘氨酸和氯甲酸苄酯为原料,合成N-苄氧羰基甘氨酸,通过正交实验考察工艺条件对反应的影响。结果表明,最佳工艺条件为:底物摩尔比n(甘氨酸)∶n(氯甲酸苄酯)=1∶1,反应时间2 h,反应温度20℃,反应液pH值为9,收率90.2%。此法反应条件温和,操作简单,收率良好。     

O-2,4-二氯苯甲基羟胺盐酸盐的合成

以丁酮肟和2,4-二氯氯苄为原料合成了O-2,4-二氯苯甲基丁酮肟醚,再用盐酸水解得到了O-2,4-二氯苯甲基羟胺盐酸盐。文章系统研究了反应温度、不同溶剂、溶剂含水量等各种实验因素对O-2,4-二氯苯甲基丁酮肟醚合成的影响,研究了盐酸浓度、原料配比等因素对O-2,4-二氯苯甲基丁酮肟醚水解工艺的影响。两步收率最高分别为94.5%和85.0%。产物熔点为167.7～169.9℃。     

甜菜碱盐酸盐的合成方法研究

以氯乙酸和三甲胺为原料,在N,N-二甲基甲酰胺(DMF)溶剂中通过季铵化反应,得到了标题化合物,经IR、1HNMR和元素分析等方法对其结构进行了表征。探讨了溶剂选择、原料配比和反应温度、时间等因素对该反应的影响,其最优反应条件为:以N,N-二甲基甲酰胺为溶剂,n(三甲胺)∶n(氯乙酸)=1.7∶1,反应温度为60℃,时间为5 h,反应收率可达95%以上。该方法较好地解决了现有合成工艺存在的分离纯化难、操作复杂、产品纯度低、生产成本高等问题,提供一种合成甜菜碱盐酸盐节能环保的工艺方法。     

硫酸羟胺的合成

以二氧化硫、亚硝酸钠、氨水为原料,合成硫酸羟胺,讨论了各种反应条件对合成羟胺收率的影响。羟胺收率大于85％,工业化生产也取得了良好的重现性。     

羟胺及烷氧基胺盐酸盐绿色生产工艺探索及实践

对羟胺及烷氧基胺盐酸盐生产工艺进行了分析比较，提出了一条酮氨氧化制备酮肟一酮肟醚化一水解制备烷氧基胺盐酸盐及回用酮这样一条绿色生产工艺路线。此工艺操作条件温和，原子经济性高，收率好。以丙酮、氯甲烷为主要原料制备甲氧基胺盐酸盐，总收率可达84．6％，原子经济性达48．O％。     

A synthetic approach to pyrazole functionalized polystyrene

Summary Polystyrene containing 20 % phenyl rings functionalized with pyrazole was obtained by acylation and subsequent reaction with N,N-dimethylformamid dimethylacetal and hydrazine and characterized by means of NMR and IR spectroscopy and elemental analysis.     

A practical approach to the development of a synthetic Gecko tape

This paper describes the fabrication and the assessment of the adhesion of bio-mimetic Gecko hair arrays. These were fabricated using photolithographic methods of the type employed in the semiconducting industry and nano-moulding using silicon moulds. Specimens comprising mushroom shaped hairs were fabricated in polyimide and polydimethylsiloxane (PDMS), and also uniform cylinder shaped hairs were made in PDMS. Contact and separation distance between the hair surface and glass surfaces was assessed via the use of optical interferometry. Adhesion strength measurements were made using a simple, purpose-built balance. Multiple attachments were achieved on a range of surfaces including glass, and rough and smooth painted surfaces. Maximum loads were recorded for the mushroom shaped PDMS specimens on glass surfaces with strengths of up to 220 kPa. PDMS based structures were also found to exhibit time dependent adhesion strengths, and also adhesion strength which was a function of the number of reattachments. The mushroom shaped structures showed adhesion on glass with a contribution from molecular and atmospheric components. The material showed superhydrophobic properties. Cleaning experiments showed that simply washing with water could recover strengths after contamination with dust and foreign hairs.     

Improved spin finish for synthetic fibres: A new approach to solving the problem

Based on an analysis of recent publications, a conclusion was drawn concerning the practical impossibility of creating multicomponent colloidal spin finishes with a defined level of processing properties. It was hypothesized that the principal solution of the problem of creating spin finishes for synthetic fibres consists of changing to the use of aqueous solutions of low-melting, ionogenic, film-forming polymers capable of large irreversible tensile strains at the temperature of orientational drawing and texturing of the fibres. Ivanovo State University of Chemistry and Technology. Translated fromKhimicheskie Volokna, No. 3, pp. 66–70, May–June, 2000.     

一种新型含咪唑基壳聚糖衍生物的合成方法和吸附性能研究

本文发现了一种合成新型氨基螯合物——N-4(5)-甲基咪唑壳聚糖(IMC),本文还通过凝胶合成法直接对4(5)-羟甲基咪唑的羟基进行取代。以上所得聚合物的结构均通过核磁共振确定。实验中,我们将样品分别与表氯醇、乙二醇缩水甘油醚、二乙二醇缩水甘油醚交联,并对吸附作用进行了研究。我们得到以下结论:聚合物的吸附作用和溶胀度取决于交联剂及其交联度;IMC对AuIII、PtIV和PdII离子的吸附作用高于非改性聚合物;随着交联度的增加,IMC从氯化物溶液中提取贵金属离子的过程变得更加有选择性;IMC对Co II和Ni II离子的吸附能力高于壳聚糖及其N杂环衍生物。     

N-benzyl-N-ethylaniline; an alternative synthetic approach

An alternative one-pot synthesis of N-benzyl-N-ethylaniline, an important dyestuff intermediate, has been achieved by reductive alkylation of easily available aniline as starting material. The reaction has been extended to the preparation of other substituted N-benzyl-N-ethylanilines. New insights into the mechanism of the reactions have been obtained. A more economical two-stage process involving reductive ethylation of N-benzylaniline has been examined.     

A new synthetic approach to asymmetric amphiphilic ABA′ block copolymers by ATRP and click reactions

Well‐defined asymmetric amphiphilic ABA′ block copolymers composed of poly(ethylene oxide) monomethylene ether (MPEO) with different molecular weights as A or A′ block and poly(styrene) (PS) as B block were synthesized by the combination of atom transfer radical polymerization (ATRP) and click reactions. First, bromine‐terminated diblock copolymer poly(ethylene oxide) monomethylene ether‐block‐poly(styrene) (MPEO‐PS‐Br) was prepared by ATRP of styrene initiated with macroinitiator MPEO‐Br, which was prepared from the esterification of MPEO and 2‐bromoisobutyryl bromide. Then, the azido‐terminated diblock copolymers MPEO‐PS‐N₃ were prepared through the bromine substitution reaction with sodium azide. Propargyl‐terminated MPEO with a different molecular weight was prepared under the basic condition from propargyl alcohol and p‐toluenesulfonyl‐terminated MPEO, which was prepared through the esterification of MPEO and p‐toluenesulfochloride using pyridine as solvent. Asymmetric amphiphilic ABA′ block copolymers, with a wide range of number–average molecular weights from 1.92 × 10⁴ to 2.47 × 10⁴ and a narrow polydispersity from 1.03 to 1.05, were synthesized via a click reaction of the azido‐terminated diblock copolymers and the propargyl‐terminated MPEO in the presence of CuBr and 1,1,4,7,7‐pentamethyldiethylenetriamine (PMDETA) catalyst system. The structures of these ABA′ block copolymers and corresponding precursors were characterized by NMR, IR, and GPC. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

A new synthetic route to 2-boratanaphthalenes

Double kaliation of 1-isopropenyl-2-methylbenzene (4) and subsequent ring closure with BCl₂(NR₂) (R=Me, iPr) provides a new and efficient access to 1,2-dihydro-2-boranaphthalenes 6′ and, after metalation with LDA in Et₂O or with LiN(SiMe₃)₂ in hexane, to lithium 2-boratanaphthalenes 7. The substituent at boron may be modified. Treatment of the B-dialkylamino compounds with BCl₃ affords the highly reactive β-chloro derivative 6c′, and subsequent methylation with ZnMe₂ in toluene affords the B-methyl compound 6d′. The lithium 2-boratanaphthalenes 7 readily form transition metal complexes such as Cp^*Fe(4-MeC₉H₆BNMe₂) (9) and Cp^*ZrCl₂(4-MeC₉H₆BMe) (10) with hexahapto coordination of the metal to the boron-containing ring.     

A new approach to investigation of nickel defect transformation in the HPHT synthetic diamonds using local optical spectroscopy

The analysis of spatial photoluminescence distribution along a plate from synthetic diamond as grown at 1500 °C allowed us to study a sequence of formation of nitrogen–nickel optically active centers and to build maps in some cases. Several groups of vibronic systems with specific spatial distribution along the sample were separated: nitrogen-vacancy pairs in the thin near- surface layer, low-temperature centers with blue emission, nickel–nitrogen complexes with a single nickel ion and those with several nickel ions.     

A new synthetic approach and biological evaluation of novel phenothiazines bearing tert-butyl group

A new and facile synthetic route is proposed for the synthesis of some novel phenothiazines (5a–5g) based on the reaction of 2-amino substituted benzenethiols with p-tert-butyl phenol in good yield. The newly synthesized compounds were characterized by IR, ¹H NMR and mass spectral studies. Their antimicrobial activities against three strains of bacteria: Bacillus subtilis, Bacillus megaterium, Escherichia coli, and two strains of fungi: Aspergillus niger and Aspergillus oryzae, were investigated.