偶合化学发光法测定血清中亚硝酸盐

采用正交试验法建立了Ｌｕｍｉｎｏｌ－ＮＯ－２－Ｋ４［Ｆｅ（ＣＮ）６］偶合发光体系测定血清ＮＯ－２的方法。本法测定ＮＯ－２的线性范围为９．０×１０－６～１．０×１０－３μｇ／Ｌ,检出限３．５×１０－６μｇ／Ｌ。对１．０×１０－４μｇ／ＬＮＯ－２连续测定１１次的相对标准偏差为２．３％。用于血清中亚硝酸根的测定,结果满意。     

STRUCTURAL MODIFICATION OF 11－ISOPROPYLIDENE endo－TRICYCLO［6．2．1．0~（2，7）］UNDECA－4， 9－DIENE－3，6－DIONE TO IMPROVE THE STABILITY

ＳＴＲＵＣＴＵＲＡＬＭＯＤＩＦＩＣＡＴＩＯＮＯＦ１１－ＩＳＯＰＲＯＰＹＬＩＤＥＮＥｅｎｄｏ－ＴＲＩＣＹＣＬＯ［６．２．１．０￣（２，７）］ＵＮＤＥＣＡ－４，９－ＤＩＥＮＥ－３，６－ＤＩＯＮＥＴＯＩＭＰＲＯＶＥＴＨＥＳＴＡＢＩＬＩＴＹ￥ＸｉａｏＰｅｉＧ...     

微波炉溶样恒温平台石墨炉原子吸收光谱法直接测定沉积物中痕量铍

研究了家用微波炉在自制的聚四氟乙烯密闭容器内,混酸（ＨＮＯ３２ｍｌ,ＨＦ２ｍｌ）分解样品,５ｇ．Ｌ＾－１Ａｌ（ＮＯ３）３作改进剂,直接定容后,在大量氢氟酸存在下,恒温平台石墨炉（ＳＴＤＰＦ）原子吸收光谱法测定水系沉积物中痕量铍。Ａｌ（ＮＯ３）３的存在,将铍的灰化温度提高到１６００℃,且消除溶解所引入的大量剩余氢氟酸干扰。方法快速、简捷、灵敏度高,再现性好,其检出限（３Ｓ）为０．１６ｎｇ．ｇ＾－１,铍的特征质量为０．７３ｎｇ／０．００４４Ａ,铍含量为１．１μｇ．ｇ＾－１的样品,取１０份同时测定,平均值为１．１６μｇ．ｇ＾＆－１,相对标准偏差为２．７７％。     

STUDIES ON THE SYNTHESIS OF TRACHYLOBAGIBBERELLINANALOGUE(Ⅱ)SYNTHESIS OF DIMETHYLESTER OF 3-HYDROXY-△1_10-12,16-CYCLOGIBBERELLIN 12

ＳＴＵＤＩＥＳ　ＯＮ　ＴＨＥ　ＳＹＮＴＨＥＳＩＳ　ＯＦ　ＴＲＡＣＨＹＬＯＢＡＧＩＢＢＥＲＥＬＬＩＮＡＮＡＬＯＧＵＥ（Ⅱ）ＳＹＮＴＨＥＳＩＳ　ＯＦ　ＤＩＭＥＴＨＹＬＥＳＴＥＲ　ＯＦ　３－ＨＹＤＲＯＸＹ－△１_１０－１２，１６－ＣＹＣＬＯＧＩＢＢＥＲＥＬ?..     

OZONOLYSIS OF 4－ISOPROPYLIDENEPENTACYCLO（5．4．0．0~（2，6）．0~（3，10）．0~（5，9））UNDECANE－8，11－DIONE

ＯＺＯＮＯＬＹＳＩＳＯＦ４－ＩＳＯＰＲＯＰＹＬＩＤＥＮＥＰＥＮＴＡＣＹＣＬＯ（５．４．０．０￣（２，６）．０￣（３，１０）．０￣（５，９））ＵＮＤＥＣＡＮＥ－８，１１－ＤＩＯＮＥ￥ＪｉａｎＧｕａｎｇＳＵＮ；ＺｈｕａｎｇＳＵ；ＹｏｎｇＺｈｏｎｇＹＵ（Ｃ...     

SYNTHESTS OF 5-SUBSTITUTED PHENYLAMINO 6-PHENY-1. 2. 4-TRIAINE-3-ONES

ＳＹＮＴＨＥＳＴＳ　ＯＦ　５－ＳＵＢＳＴＩＴＵＴＥＤ　ＰＨＥＮＹＬＡＭＩＮＯ　６－ＰＨＥＮＹ－１．２．４－ＴＲＩＡＩＮＥ－３－ＯＮＥＳ￥ＺｈｏｎｇＥＬＵ；ＷｅｎＱｉｎＺＨＥＮＧ；ＲｕｎＳｈｅｎｇＺＥＮＧ；ＪｉａｎＰｉｎＺＨＯＵ；ＫｅＱｉａｎＣＨＥＮ（...     

SYNTHESIS AND CHARACTERIZATION OF NOVEL FUNCTIONAL HOST COMPOUNDS 1．MONO－（6－ANILINO－β－CYCLODEXTRIN）

ＳＹＮＴＨＥＳＩＳＡＮＤＣＨＡＲＡＣＴＥＲＩＺＡＴＩＯＮＯＦＮＯＶＥＬＦＵＮＣＴＩＯＮＡＬＨＯＳＴＣＯＭＰＯＵＮＤＳ１．ＭＯＮＯ－（６－ＡＮＩＬＩＮＯ－β－ＣＹＣＬＯＤＥＸＴＲＩＮ）￥ＹｕＬＩＵ；ＹｉＭｉｎＺＲＡＮＧ；ＹｕｎＴｉＣＨＥＮ（Ｄｅｐａｒｔ...     

A CONVERGENT SYNTHESIS OF（E．E，E）－3，7，13－TRIMETHYL－6－（i－PROPENYL）－7，14－DIHYDROXY－2，8，12－TETRADECATRIEN－1－METHYLAL

ＡＣＯＮＶＥＲＧＥＮＴＳＹＮＴＨＥＳＩＳＯＦ（Ｅ．Ｅ，Ｅ）－３，７，１３－ＴＲＩＭＥＴＨＹＬ－６－（ｉ－ＰＲＯＰＥＮＹＬ）－７，１４－ＤＩＨＹＤＲＯＸＹ－２，８，１２－ＴＥＴＲＡＤＥＣＡＴＲＩＥＮ－１－ＭＥＴＨＹＬＡＬ￥ＹｉｑｉａｎＷａｎ；ＪｉｎｇＹ...     

THE SYNTHESIS AND CRYSTAL STRUCTURE COMPLEX OF SCHIFF BASE CONTAINING S·N－Cd_3｜CH_3O（O）C_6H_3CH＝NNHC（S）NH_2｜4·（CH_3COO_2·1／2［CH_3S（O）CH_3］·2H_2O

ＴＨＥＳＹＮＴＨＥＳＩＳＡＮＤＣＲＹＳＴＡＬＳＴＲＵＣＴＵＲＥＣＯＭＰＬＥＸＯＦＳＣＨＩＦＦＢＡＳＥＣＯＮＴＡＩＮＩＮＧＳ·Ｎ－Ｃｄ_３｜ＣＨ_３Ｏ（Ｏ）Ｃ_６Ｈ_３ＣＨ＝ＮＮＨＣ（Ｓ）ＮＨ_２｜４·（ＣＨ_３ＣＯＯ_２·１／２［ＣＨ_３Ｓ（Ｏ）ＣＨ_３］·?..     

亚硝酸根—巯基乙酸—钴（Ⅱ）络合物的极谱吸附波研究

提出了一个测定痕量亚硝酸根的极谱吸附波新体系．在含有巯基乙酸（ＴＧＡ）和钻．（Ⅱ）的 ｐＨ ４．４的 Ｈ２ＳＯ４－ＮａＡｃ介质中，得到一灵敏的亚硝酸根络合物单扫极谱吸附波，峰电位为－０．７５ Ｖ（ｖｓ．ＳＣＥ）．峰电位与亚硝酸根浓度在１．１× １０－３－８．７×１０－６ｍｏｌ／Ｌ范围内呈线性关系．检出限为 ５． ５×１０－９ ｍｏｌ／Ｌ．本法简便快速，选择性好，用于水样和食品中痕量ＮＯ-２的测定，结果满意。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.