The Reaction of Diethanolamine with 2-Chloronitrobenzene-A Reinvestigation

In a report on the reaction of 2-chloronitrobenzene (1) with diethanolamine (2), Meltsner et al ¹ claim that the expected S_NAr product, N-(2-nitrophenyl)diethanolamine (3), is not formed; rather that the products are 2,2′-dichloroazobenzene (4), 2-nitrophenol (5), 2-chloroaniline (6) and 4-(2-aminophenyl)morpholine (7). Similar products in which the nitro function is reduced are also reported² for the corresponding reaction with ethanolamine. In this laboratory, in an attempted preparation of 2,2′-dichloroazobenzene (4) for reference purposes in photochemical studies on the antineoplastic agent 5-(3-azido-4-chlorophenyl)-6-ethyl-pyrimidin-2,4-diamine³, the expected S_NAr product (3) was obtained along with other products.     

A Reinvestigation of the Reaction of Hmpa With Ketoximes

A series of ketoximes have been found to react with HMPA in the absence of acid catalysis to produce N,N-dimethyl-N′-arylamidines in reasonable yields.     

A Reinvestigation of the Reaction of Hydrazine Hydrate With 2-Substituted Styryl-4-Quinazolones

The reaction of hydrazine hydrate with certain 2-substituted styryl-4-quinazolones results in the formation of a novel tricyclic heterocycle and not the previously reported acyl hydrazide. A mechanistic rationale is presented.     

2-[2′-苯并噻唑偶氮]-1,8-二羟基萘-3,6-二磺酸的合成及与铝的显色反应研究

本文合成了新的显色试剂2-〔2’-苯并噻唑偶氮〕-1,8-二羟基萘-3,6-二磺酸,并研究了与铝的显色反应.在CTMAB存在下,铝与试剂于pH7.0～8.0的缓冲溶液中形成稳定的深紫红色络合物,组成为Al(Ⅱ):R=1:2表观摩尔吸光系数为1.46×10~5L·mol_(-1)·cm~(-1).铝浓度在0～5.0 μg/25mL范围内符合比尔定律.该方法灵敏度高,选择性好,并用于测定低合金钢、稀土硅镁合金和硅铁等试样中的微量铝.     

On the Reaction of 2-Benzylamino-1,4-naphthoquinones with Nitrosylsulfuric Acid

Russian Journal of Organic Chemistry - The reaction of 2-benzylamino-1,4-naphthoquinone with nitrosylsulfuric acid in acetic acid results in preferential formation of 2,1- and 2,3-heterocyclization...     

A Convenient Synthesis of 3,6-Anhydro-2-deoxy-D-glucose [Isoglucal] and Some of Its Derivatives

Abstract

The present paper describes a facile synthesis of isoglucal (3,6-anhydro-2-deoxy-D-glucose, 3), starting from the easily available α,β-unsaturated aldehyde (2E)-4,6-di-O-acetyl-2,3-didehydro-aldehydo-D-erythro-hex-2-enose (1). Compound 3 exists in equilibrium with its corresponding bicyclic forms whose anomeric configurations and ring-sizes have been determined.     

2-〔2′-(6-溴-苯并噻唑)-偶氮〕-1,8-二羟基萘-3,6-二磺酸的合成及其与钛的显色反应

本文合成了一种新的革并座隆类显色试剂—2－［2′－（6－溴－苯并噻唑）－偶氮］－1，8－二羟基萘－3，6－二磺酸（简称Br－BTCA），并研究了其与钛的显色反应。在CTMAB存在下，钛与试剂形成稳定的络合物，其ε616=1．15×105L·mol－1·cm-1，组成为Ti（Ⅳ）：R：=1：2：钛浓度在0～0．5mg／L范围内符合比尔定律，该方法灵敏度高，选择性好，并用于铝合金及硅铁试样中微量钛的测定     

Kinetic Model For The Reaction of Ilmenite With Sulphuric Acid

The kinetic of the reaction ilmenite with sulphuric acid was studied using non-adiabatic and non-isothermic calorimetric device system. The kinetic model based on interphase surface and kinetic models found in literature which are usually applied were tested. The best agreement between experimental and calculated values was found with model based on first order of reaction and model of contracting volume. This revised version was published online in July 2006 with corrections to the Cover Date.     

1,4—二巯基苏糖醇与磷钼黄的反应机理及该反应的分析意义

在ＰＨ４的邻苯二甲酸氢钾缓冲溶液中，１，４－二巯基苏糖醇可较快地将磷钼黄还原成磷钼蓝。该反应对ＤＴＴ为准一级反应，反应中ＤＴＴ分子的两个巯基各失去一个电子，巯基失电子后相互结合成双硫链。该反应能定量进行，因此可用于ＤＴＴ的间接光度测定，应用此方法测定ＤＴＴ的适用范围为２．０×１０＾－６－１．０×１０＾－４ｍｏｌ／Ｌ。     

The Reaction of 2-Methylindole with Pyruvic Acid

The reaction of 2-methylindole with pyruvic acid was studied. Two products are found to be depending on experimental conditions, including the 2:2 condensation adduct and the 2:1 condensation adduct. The reaction mechanism evidently involves a 1:1 adduct of 2-hydroxy-2-(2-methylindol-3-yl)-propionic acid as an intermediate.     

Self-Assemblies of Extended Hydrogen-Bonded Arrays Using 1,4-Butanebisphosphonic Acid as a Versatile Building Block

Two organic salts of 1,4-butanebisphosphonic acid, bis(ethylenediammonium) butanebisphosphonate hydrate ( 1 ) and bis(hexamethylenediammonium) butanebisphosphonate hydrate ( 2 ), have been structurally characterized using single-crystal x-ray diffraction analyses. Compound 1 exhibits a H-bonded pillared bilayered structure, in which etheylenediammonium cation acts as a spacer between the anions resulting in the formation of two types of cavities. The larger cavity is filled by four water molecules though having hydrophobic character. Thus, the material behaves as a nanoporous organic solid. Compound 2 shows a multidimensional hydrogen bonding networks: one-dimensional arrays parallel to the b axis and two-dimensional sheets parallel to the ab plane. The N--H·;·;·;O--P hydrogen bonds, forming H-bonded supramolecular networks, are regarded to be strong and directional hydrogen bonds.     

铁-过氧化氢-变色酸催化动力学光度法测定痕量铁

本文研究了在H3PO4介质中，痕量铁（Ⅲ）催化过氧化氢氧化变色酸的褪色指示反应及最佳实验条件条件和动力学参数，建立了测定痕量铁的新方法。方法的灵敏度为6．18×109g／L；测定范围0～30μg／L。用于各种水平痕量铁的测定获得满意结果。     

Photolysis of 2-(Triorganostannyloxy)-3,6-di-tert-butyl-benzquinone-1,4 in Alkanes Solution

Abstract

Photolysis of 2-(trimethylstannyloxy)-3,6-di-tert-butyl-benzquinone-1,4 (I), 2-(triphenylstannyloxy)-3,6-di-tert-butyl-benzquinone-1,4 (II), and 2-(tribenzylstannyloxy)-3,6-di-tert-butyl-benzquinone-1,4 (III) by light with the wavelength 436 nm leads to the evolution of carbon mono- and dioxide and the formation of hydrocarbon radicals with their consequent recombination.

GRAPHICAL ABSTRACT     

新显色剂2-[2-噻唑偶氮]-5-二乙氨基苯甲酸与铑显色反应的研究

本文合成了新显色剂2-[2-噻唑偶氮]-5-二乙氨基苯甲酸(TAEB),研究了它与铑的显色反应。结果发现,在pH4.0～6.5的缓冲溶液中,铑(Ⅱ)与TAEB形成一种绿色络合物。其最大吸收波长为674nm,表现摩尔吸光系数为1.44×10~5L·mol~(-1)cm~(-1)。铑含量在0～20μg/25ml范围内服从比尔定律。络合物中铑(Ⅱ)与TAEB的摩尔比为1:1。该方法灵敏度高、选择性好。常见的阴、阳离子不干扰,镍(Ⅰ)、钴(Ⅰ)和铜(Ⅰ)的干扰可用EDTA来消除,用于催化剂中微量铑的测定。结果令人满意。     

Synthesis of 2,5-bis(2-aminothiazol-5-yl)-3,6-dichloro-1,4-benzoquinones

A series of 2-(2-aminothiazol-5-yl)-3,6-dichloro-5-diethylaminoethenyl-1,4-benzoquinones was synthesized from 2-(2-aminothiazol-5-yl)-3,5,6-trichloro-1,4-benzoquinones using acetaldehyde and diethylamine in toluene solution. Refluxing these compounds with substituted thioureas in acetonitrile in the presence of hydrochloric acid gives the corresponding 2,5-bis(2-aminothiazol-5-yl)-3,6-dichlorohydroquinones which can be oxidized to the target products with ferric chloride in aqueous DMF.Riga Technical University, Riga LV-1048, LatviaTranslated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 835–839, June, 2000     

Synthetic Studies on 2H-Thiopyran Compounds: A Reinvestigation of the Reaction Between Benzaldehydes and Sodium Sulfide

An investigation regarding the synthesis of 2H-thiopyran compounds from substituted benzaldehydes with sodium sulfide (Na₂S·10H₂O) in aqueous ethanol was carried out. The structural elucidation of the products was performed by spectroscopic methods and in one example as X-ray crystallographic analysis. A plausible mechanistic pathway is also proposed that is entirely different from an earlier report.     

The Reaction of the cis-ReO2 + Core with 2-Amino-3-Methylbenzoic Acid

The reaction of a twofold molar excess of 2-amino-3-methylbenzoic acid (H₃amb) with cis-[ReO₂I(PPh₃)₂] in ethanol led to the isolation and characterization of the six-coordinate [Re(amb)(OEt)I(PPh₃)₂] (1). The X-ray crystal structure of 1 illustrates that the trianionic ligand amb acts as a bidentate chelate via the doubly deprotonated amino nitrogen, which is present in 1 as an imide, and the deprotonated acetoxy oxygen. The Re=N bond length is 1.751(3)?Å, and the Re=N–C angle [143.6(3)°] deviates considerably from linearity.