Synthesis of Spiropyrimidodiazepines and Spirodiazepinopurines by Tandem Nitroso‐ene/Diels–Alder Reactions

New spirocyclic heterocycles 8, 16, 19/20, 25, 27 , and 30 derived from pyrimido[4,5‐b][1,4]diazepin]‐8′(9′H)‐one were synthesised by a tandem nitroso‐ene/Diels–Alder reaction of 4‐(alkenoylamino)‐5‐nitrosopyrimides. The crystal structure of 16 was established by X‐ray analysis. It is characterised by four pairs of intermolecular H‐bonds linking every two molecules in the unit cell. Sequential imine reduction and intramolecular condensation of the C(4′)‐(acylamino)‐pyrimido[4,5‐b][1,4]diazepines 27 and 30 led to the [1,4]diazepino[1,2,3‐gh]purines 28 / 29 and 31 , respectively.     

Recent Advances in Rare‐Earth Polypnictides

The polypnictide complexes of rare earth cations have drawn the attention of the scientific community for their uncommon bonding modes and potential applications. Herein, we present a systematic and comprehensive summary on recent advances in the field of rare earth polypnictides, focusing on their synthesis, structures, and reactivities. The structural stabilizing effects imposed by the electropositive rare earth cations as well as the reducing capability of rare earth precursors in the synthesis of these polypnictide complexes are described in this review. We also disscuss in detail the bonding interactions and coordination modes between rare earth cations and polypnictide clusters as well as the similarities and the peculiarity of some structures.     

离子液体中用Heck反应合成2-取代萘烯丙醇化合物

利用Heck反应, 在离子液体、金属钯或镍、碱和膦配体反应体系中, 由卤代萘与烯丙醇反应, 制得了高收率和高选择性的2-取代萘烯丙醇化合物. 该方法原料便宜易得、操作简单、反应体系可循环使用. 并讨论了醋酸镍替代醋酸钯、不同膦配体、溶剂及碱对反应转化率的影响. 通过核磁共振、红外光谱、质谱和元素分析对产物的结构进行了表征.     

High-throughput purification of combinatorial libraries I: a high-throughput purification system using an accelerated retention window approach

We have developed a high-throughput purification system to purify combinatorial libraries at a 50-100-mg scale with a throughput of 250 samples/instrument/day. We applied an accelerated retention window method to shorten the purification time and targeted one fraction per injection to simplify data tracking, lower QC workload, and simplify the postpurification processing. First, we determined the accurate retention time and peak height for all compounds using an eight-channel parallel LC/UV/MS system, and calculated the specific preparative HPLC conditions for individual compounds. The preparative HPLC conditions include the compound-specific gradient segment for individual compounds with a fixed gradient slope and the compound-specific UV or ELSD threshold for triggering a fraction collection device. A unique solvent composition or solvent strength was programmed for each compound in the preparative HPLC in order to elute all compounds at the same target time. Considering the possible deviation of the predicted retention time, a 1-min window around the target time was set to collect peaks above a threshold based on UV or ELSD detection. Dual column preparative instruments were used to maximize throughput. We have purified more than 500 000 druglike compounds using this system in the past 3 years. We report various components of this high-throughput purification system and some of our purification results.     

Thermodynamic and Equilibrium Composition Analysis of Using Iron Oxide as an Oxygen Carrier in Nonflame Combustion Technology

1. Introduction The utilization of fossil fuels causes serious neg- ative impacts on the environment and human life. There are many pollutants such as SOx, NOx and CO2 emission produced from the combustion of coal, oil and natural gas. It has been known for more than 100 years that CO2 is a greenhouse gas and that the release of CO2 from fossil fuel combustion may affect the climate of the earth. In the last years the concern over the aspects of an increased release of greenhouse gases has…     

四价锗与3, 4－二羟墓苯甲醛配合物的极谱研究

本文采用极谱法研究了Ge(Ⅳ)-3,4-二羟基苯甲醛(DHB)配合物的组成,条件稳定常数.并对该配合物的极谱波性质进行了研究.     

Pore size distributions in low‐k dielectric thin films from X‐ray porosimetry

X‐ray reflectivity has been used to determine the mass uptake of probe molecules in porous thin films supported on thick silicon wafers. The adsorption occurs by capillary condensation when the films are exposed to probe vapor at controlled partial vapor pressures. The probe solvent partial pressure was varied by mixing saturated air and dry air at constant temperature or by changing sample temperature at a constant vapor concentration. Pore size distribution in the films can be calculated from the probe uptake with typical porosimetric approaches such as the application of the Kelvin equation to convert partial pressure into pore size. For illustration, the pore size distribution of three different nanoporous thin films, the primary candidate of ultra‐low‐k interlevel dielectrics in the next generation of integrated circuit chips, was determined with this technique. These samples represent different generations of low‐k dielectrics developed by industry. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 2170–2177, 2002     

从蓖麻油制取10-羟基癸酸的研究

本文报道了从蓖麻油制取10-羟基癸酸的研究,发现了从蓖麻油制取10-羟基癸酸的新的工艺路线和最佳的工艺条件,用氢氧化钠用量、2-辛醇量、反应时间和反应温度四因子三水平L_9(3~4)进行了正交试验,发现最佳工艺条件是:氢氧化钠(g)/蓖麻油(g):1.25:2-辛醇量(g)/蓖麻油(g):2:反应时间:6h;反应温度:180℃。在这一新的工艺路线和最佳工艺条件下,10-羟基癸酸产率可达75％。     

Extraction of Americium(III) and Europium(III) with Two Open-Chain Crown Ethers of Amide Type

The extraction of Am³⁺ and Eu³⁺ from aqueous picric acid solution by N, N-dinaphthyl-N, N-diphenyl-3,6-dioxaoctanediamide (L^I) and 1, 1-(3, 6, 9-trioxaundecanedionyl)diphenothiazine (L^II) was investigated by a radioactive tracer technique. Extraction distribution ratios of Am³⁺ and Eu³⁺ have been measured as a function of pH, picric acid concentration, extractant concentration, diluent and temperature. The extraction of Am³⁺ is preferred to that of Eu³⁺ for both L^I and L^II, and the latter gives larger separation factor than the former. The equilibrium constants and thermodynamic parameters of extraction reactions were also calculated.     

镉—溴化物—罗丹明B高灵敏显色反应的研究：离心光度法测定镉

本研究了一个高灵敏的测定镉的方法，离心光度法，该体系络合物λｍａｘ＝５６０ｎｍ，表观摩尔吸系数ε５６０＝５．０６×１０＾８Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，Ｃｄ＾２＋浓度０．１０×１０＾－２－１．０×１０＾－２μｇ／１０ｍＬ呈线性关系，本法已用于血清和水中痕量镉的测定，探讨了高灵敏的显色反应机理。