季戊四醇螺环磷酸苯酚酯的合成及结构表征

季戊四醇螺环磷酸苯酚酯的合成及结构表征;季戊四醇螺环磷酸苯酚酯;季戊四醇螺环磷酰二氯;苯酚;绿色合成     

TS-1分子筛催化苯酚和草酸二甲酯合成草酸二苯酯

碳酸二苯酯;酯交换;TS-1分子筛催化苯酚和草酸二甲酯合成草酸二苯酯     

Sn改性TS－1分子筛催化苯酚和草酸二甲酯合成草酸二苯酯

 使用Sn改性的TS－1分子筛催化苯酚和草酸二甲酯的酯交换反应合成草酸二苯酯，深入研究了不同Sn负载量TS－1分子筛的结构及催化性能．实验结果表明，由于Sn和以Ti－O－SiO3为中心的弱Lewis酸的协同催化作用，与未改性的TS－1分子筛催化剂相比，改性后的催化剂虽 然Lewis酸量有明显下降，但催化剂的催化性能明显提高．当Sn的负载量为2％时，草酸二甲酯的转化率达到50．3％，目的产物的选择性为99．2％．利用X射线衍射、X射线光电子能谱和X射线能量分散谱考察了Sn在TS－1分子筛表面的结构和分散状态及其与酯交换反应催化性能的关系．结果表明，当Sn的负载量低于2％时，SnO2以非晶态形式分散在TS－1表面；而当Sn负载量高于2％时，SnO2以微晶的形式存在，此时Sn原子与Ti原子的协同作用已经不明显，催化剂的催化性能反而下降．     

以对硝基磷酸苯酯为底物电化学分析法检测碱性磷酸酯酶

研究了对硝基磷酸苯酯（ＰＮＰＰ）为底物伏安法测定碱性磷酸酯酶（ＡＬＰ）的方法。ＰＮＰＰ在ＡＬＰ的催化作用下水解生成对硝基苯酚（ＰＮＰ）。ＰＮＰ在玻碳电极上＋１．０２Ｖ（ｖｓＡｇ／ＡｇＣｌ）左右产生氧化峰,借助此氧化电流可以测定ＡＬＰ,并进而可用于以ＡＬＰ为标记物的酶免疫分析。用微分脉冲伏安法对酶催化反应条件和酶催化反应产物的测定条件进行了详细的研究,测定ＡＬＰ的线性范围是４．０×１０２～１．０×１０６ｍＵ／Ｌ;检测限为２．８ ×１０２ｍＵ／Ｌ。     

叔丁基过氧化氢介导的磷酸硒酯合成

磷酸硒酯化合物广泛应用于有机合成和药物发现等相关领域.因此,开发高效简便合成该类化合物的新方法受到化学家的广泛关注.报道了一种以叔丁基过氧化氢(TBHP)为氧化剂,在温和的反应条件下实现了亚磷酸酯和二硒醚偶联反应制备硒代磷酸酯方法.与现有方法相比,该方法具有条件温和、底物适用范围广泛、产率高、且不需过渡金属和强碱等优点...     

氟烷基磺酸苯酯合成的改进

在三乙胺中,通过氟烷基磺酰氟与酚类化合物反应,可得到较高产率的氟烷基磺酸苯酯。这些酯部是新化合物。     

纳米Cu2O催化二苯甲烷二氨基甲酸苯酯无溶剂热分解制备二苯甲烷二异氰酸酯

研究了无溶剂条件下纳米Cu₂O催化二苯甲烷二氨基甲酸苯酯(MDPC)热分解制备二苯甲烷二异氰酸酯(MDI),考察了纳米Cu₂O的制备条件与反应条件对MDPC热分解反应性能的影响.结果表明,水解法制备的纳米Cu₂O在Ar中于300℃焙烧2h,其催化性能最佳;最佳的反应条件为Cu₂O用量为原料总重的0.06%,反应温度220℃,反应压力0.6kPa,反应时间12min,此时MDPC转化率达到99.8%,MDI选择性86.2%.     

Synthesis and characterization of novel phosphoramidates containing benzimidazole moiety

Novel heterocyclic phosphoramidates were synthesized by a nucleophilic substitution reaction of 2-substitutedbenzimidazoles and diphenyl chlorophosphate (ClPO₃Ph₂) in the presence of potassium hydroxide (KOH) under an argon atmosphere. The structures of the phosphoramidates were characterized by NMR, IR, melting point, and elemental analysis.     

Preparation of the thermotropic copoly(amide ester) of p‐aminobenzoic acid and m‐hydroxybenzoic acid with diphenyl chlorophosphate/pyridine

A thermotropic copoly(amide ester) exhibiting a nematic mesophase within the range of 240–360 °C was prepared by the solution copolycondensation of p‐aminobenzoic acid (40–70 mol %) and m‐hydroxybenzoic acid with diphenyl chlorophosphate in pyridine in the presence of LiCl. For control of the sequence distribution of p‐aminobenzoic acid, the amount of LiCl and the dropwise addition of the phosphate were examined. The transition temperatures (from a solid phase to a nematic mesophase) of the resultant copolymers were affected by the period of addition and the amounts of the aminobenzoic acid and LiCl and were investigated in terms of the distributions of the monomers determined by ¹H NMR. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 1775–1780, 2002     

双(二苯基膦)烷烃的合成与表征

以三苯基膦为起始原料,四氢呋喃为溶剂,经过金属锂化与烷基化分别合成了1,1-双二苯基膦甲烷(DPPM)、1,2-双二苯基膦乙烷(DPPE)、1,3-双二苯基膦丙烷(DPPP)、1,4-双二苯基膦丁烷(DPPB)、1,5-双二苯基膦戊烷(DPPPe)和1,6-双二苯基膦己烷(DPPH),收率为75%~86%.通过1 H NMR、31 P NMR、MS和元素分析确证了目标化合物的结构.     

多溴代双羟基二苯醚的合成与抑菌活性研究

自1981年Brad等[1]首次报道从一种名为Dysides的海洋海绵体中分离出两种天然多溴代2,2′-二羟基二苯醚以来,许多科学家对此类化合物进行了大量的研究,发现它们具有较好的抑菌杀菌能力[2],杀菌效果很好,稳定性好,毒性低,对皮肤无刺激性,无致敏性、无腐蚀性,能抑制致癌的肌苷酸脱     

氯代苯二酚双苯醚的合成与抑菌活性研究

为了寻求优良的苯醚类新化合物抑菌剂,本文设计合成了邻(对)苯二酚二-(2-氯-4-羟基苯基)醚,其结构均经1HNMR、IR、MS和元素分析证实,并且测试了化合物对大肠杆菌,金黄色葡萄球菌,白色念珠菌,白色葡萄球菌,变形杆菌,卡他双球菌,青枯假单胞菌的抑菌活性,初步研究结果表明:羟基的位置对活性存在较大影响,羟基的个数对试剂的抑菌活性没有明显的影响。     

Na2S还原法合成氨基二苯醚类化合物

氨基二苯醚不仅自身具有良好的杀菌、杀虫功效,广泛地应用到医药及农业领域。一般通过还原硝基二苯醚得到,但现有制备方法存在一些问题。Na2S作为一种较成熟的还原剂,价格低廉,反应后生成的Na2S2O3可作化工原料。本文用Na2S作为还原剂,合成路线如下：     

Synthesis of high-molecular-weight poly(amide-ester)s by direct polycondensation with diphenyl chlorophosphate

High molecular weight aromatic poly(amide-ester)s were prepared by the direct polycondensation reactions between aromatic dicarboxylic acids and aminophenols under mild conditions in pyridine. The condensing agents examined in this study were diphenyl chlorophosphate (DPCP), DPCP/LiCl, and DPCP/DMF. Addition time of the aminophenols, depending on their nucleophilicities, affected the η_inh values and monomer sequence of the resulting polymer. Their thermal properties were studied in terms of the sequences in the polymer backbones.     

Synthesis and characterization of novel pyridyl/naphthyl/(diphenyl)methylseleno substituted alkanoic acids: X-ray structure of 2-pyridylselenoethanoic acid, 2-naphthylselenoethanoic acid and 2-(diphenyl)methylselenoethanoic acid

A number of novel and synthetically important pyridyl/naphthyl/(diphenyl)methylseleno substituted alkanoic acids (20-25) have been synthesized using an efficient and operationally simple strategy. Starting substrates, ethyl pyridyl/naphthyl/(diphenyl)methylseleno substituted alkanoates (8-13) were easily prepared by treatment of ethyl chloroalkanoates 7(a-c) with nucleophilic selenium reagent RSeNa⁺, generated from the cleavage of dipyridyl/dinaphthyl/bis(diphenylmethyl) diselenide (1-6) with sodium borohydride in ethanol. The ethyl pyridyl/naphthyl/(diphenyl)methylseleno substituted alkanoates (8-13) on basic hydrolysis and subsequent acidification afford pyridyl/naphthyl/(diphenyl) methylseleno substituted alkanoic acids (20-25) in excellent yields. These selenoalkanoates (8-13) and selenoalkanoic acids (20-25) have been characterized by elemental analysis and various spectroscopic techniques viz. NMR (¹H, ¹³C and ⁷⁷Se), IR and mass spectrometry. The molecular structure of 2-pyridylselenoethanoic acid (20a), 2-naphthylselenoethanoic acid (23a) and 2-(diphenyl)methylselenoethanoic acid (24a) has also been established with the help of single crystal X-ray analysis.     

Synthesis of diphenyl[alkyl(aryl)trimethylsiioxymethyl]phosphines

A series of previously unknown diphenyl[alkyl(aryl)trimethylsiloxymethyl]phosphines was prepared by the reaction of diphenyl(trimethylsilyl)phosphine with carbonyl compounds. The first complexes of these ligands with palladium chloride were prepared.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 754–756, April, 1994.