Solvent-Free Synthesis of Core-Functionalised Naphthalene Diimides by Using a Vibratory Ball Mill: Suzuki,Sonogashira and Buchwald–Hartwig Reactions

Solvent-free synthesis by using a vibratory ball mill (VBM) offers the chance to access new chemical reactivity, whilst reducing solvent waste and minimising reaction times. Herein, we report the core functionalisation of N,N’-bis(2-ethylhexyl)-2,6-dibromo-1,4,5,8-naphthalenetetracarboxylic acid (Br₂-NDI) by using Suzuki, Sonogashira and Buchwald–Hartwig coupling reactions. The products of these reactions are important building blocks in many areas of organic electronics including organic light-emitting diodes (OLEDs), organic field-effect transistors (OFETs) and organic photovoltaic cells (OPVCs). The reactions proceed in as little as 1 h, use commercially available palladium sources (frequently Pd(OAc)₂) and are tolerant to air and atmospheric moisture. Furthermore, the real-world potential of this green VBM protocol is demonstrated by the double Suzuki coupling of a monobromo(NDI) residue to a bis(thiophene) pinacol ester. The resulting dimeric NDI species has been demonstrated to behave as an electron acceptor in functioning OPVCs.     

在H型分子筛上萘与正己醇的烷基化反应

制备了H型分子筛HY,Hβ和HM,通过XRD,NH₃-TPD和Py-IR对其进行了表征,考察了其对萘与正己醇的烷基化反应的催化性质.结果表明,HY可作为己基化反应的催化剂,较高的反应温度和较长的反应时间对β-己基萘的生成有利.     

含双萘环通用染料的合成与染色性质

含双萘环通用染料的合成与染色性质;通用染料;双萘环;合成;染色     

微晶萘负载PMBP微柱分离预富集与电热蒸发-电感耦合等离子体原子发射光谱联用测定痕量稀土元素

报道了微晶萘负载1-苯基-3-甲基-4-苯甲酰基-5-吡唑酮(PMBP)微型柱分离预富集与电热蒸发-电感耦合等离子体原子发射光谱(ETV-ICP-AES)联用测定痕量稀土元素(Sc,Y,La和Yb)的新方法.试验了影响分离/预富集待测物的各种因素(包括溶液酸度、流速、试样体积、微柱尺寸);研究了吸附有待测物的微晶萘的溶解方法及共存元素对分离/测定的影响.在优化的实验条件下,方法的相对检出限为14pg/mL(Sc),32pg/mL(Y),190pg/mL(La)和26pg/mL(Yb),相对标准偏差(RSD)分别为3.1%,3.5%,4.8%和3.4%(n=9,c=10ng/mL).本法已成功地应用于生物样品中痕量稀土元素(Sc,Y,La和Yb)的测定,结果满意.     

微波萃取/GC-MS法对电子电气产品中多氯萘的测定

建立了微波萃取/GC-MS法检测电子电气产品中多氯萘的方法。将破碎后的样品以甲苯为溶剂进行微波萃取,萃取液经硅胶小柱净化、平行蒸发定量浓缩后采用气相色谱-质谱法测定多氯萘的含量,外标法定量。优化了样品前处理条件,包括前处理方式、微波萃取溶剂、萃取时间,以及净化小柱的选择。对于8种含不同氯原子数的多氯萘,在1~50 mg/L范围内,线性关系良好,相关系数均大于0.995;方法定量下限为0.2~1.0 mg/kg,相对标准偏差为2.7%~7.2%,回收率为77%~112%。该法操作简便、分析迅速、结果准确,可以满足对电子电气产品中多氯萘的定性确证和定量分析。     

An HPLC method for the determination of selected amino acids in human embryo culture medium

A method for the determination of selected amino acids in culture medium using HPLC with fluorescence detection is described. Twenty hours after intra‐cytoplasmic sperm injection, one randomly selected zygote was transferred to the culture medium. After incubation (72 h after fertilization), the culture medium in which the embryo was incubated and blank medium was immediately stored at −80°C. Filtered medium samples were derivatized with ortho ‐phthalaldehyde (naphthalene‐2,3‐dicarboxaldehyde), forming highly fluorescent amino acids derivatives. Reverse‐phase columns (LichroCART, Purospher STAR RP_18e or Ascentis Express C₁₈) were used for the separation. The derivatives were analyzed by gradient elution with a mobile phase containing ethanol and sodium dihydrogen phosphate. The analytical performance of this method is satisfactory for all amino acids; the intra‐assay coefficients of variation were <10% and quantitative recoveries were between 95.5 and 104.4%. Changes in the levels of selected amino acids before and after human embryo cultivation were observed. After embryo incubation, the levels of all amino acids in the medium were increased, apart from aspartate and asparagine. After the cultivation of some embryos, amino acids which were not part of the medium were detected. Low amino acids turnover was observed in some embryos.     

1,2,1′,2′-双蒽醌-3,12-二羧酸的还原反应

1,2,1＇,2＇-双蒽醌-3,12-二羧酸(1)是一个π-共轭体系芳环化合物,内环酮基由于受空间效应和共振效应的影响,不能被还原成相应的醇或相应的碳氢基团,却成了不常见的内“双氧桥”化合物(4)。化合物2,3,4的结构已经确定,并对1的还原机理进行了初步讨论。     

Simultaneous emissions from T2 and T1 states of naphthalene moiety in a specially designed naphthalene cryptand

We report here the photophysical properties of a naphthalene derivative of a specially designed cryptand system (L). The system exhibits the unusual phenomenon of emission from T₂ and T₁ states of naphthalene which has been attributed to the inherent rigidity of the system. The results obtained have been analysed by comparison with two other model systems where the flexibility of the fluorophore unit with respect to the receptor moiety have been varied.     

交联萘沥青的组成与结构特征

萘与硫在较低温度下交联聚合，制得了可溶性好、残炭值高、软化点较低，流动性良好的交联萘沥青。结构分析发现，此沥青分子量分布较窄，主要由三到四个萘分子交联而成，推测其反应机理，估计聚合物经萘环侧位交联成环而形成长链状硫杂环类结构。