Dicholorbenzyl alkyl ether homologs as retention index markers and internal standards for the analysis of environmental samples using capillary gas chromatography

A homologous series of 2,4-dichlorobenzyl alkyl ethers (DCBEs) have been synthesized and purified for use as retention index calibrants and internal standards. They are stable, sensitive to ECD and FID and ideal for GC-MS, with base peaks at m/z 159/161. The retention index calibration against the n-alkanes for a linear temperature program (LTP) series is given and recommendations made for the most suitable members of the DCBE series for use as internal standards in organochlorine (OC) residue analysis.     

N-烷基壳聚糖衍生物的合成及其对阳离子的吸附性能

烷基衍生物;阳离子吸附性能;N-烷基壳聚糖衍生物的合成及其对阳离子的吸附性能     

Synthesis of 4‐Alkyl‐1(2H)‐phthalazinones and 4‐Alkyl‐2,3‐benzoxazin‐1‐ones via Ring Cleavage of 3‐Substituted N‐Alkylated‐3‐hydroxyisoindolin‐1‐ones

Abstract

N‐Alkyl (Me, Et, i‐Pr, t‐Bu)‐substituted phthalimdes 5a–d were easily transformed to 1(2H)‐phthalazinones 8d–i and 2,3‐benzoxazin‐1‐ones 9d, f, and j via a one‐pot addition–decyclization–cyclocondensation process.     

A Rapid and Facile Esterification of Na-Carboxylates with Alkyl Halides Promoted by the Synergy of the Combined Use of DMSO and an Ionic Liquid Under Ambient Conditions

The synergy of the combined use of DMSO and an ionic liquid viz. (bbim)⁺Br^? has brought about a rapid and efficient esterification of sodium carboxylates with acyl and alkyl halides under ambient conditions in excellent isolated yields (90–95%) in short reaction times (12–40 min).     

Synthesis of (22R, 25R)-3β,26-Dihydroxy-5α-furostan-6-one #

The synthesis of a plant growth promoter furostanol which bears the characteristic functionality of teasterone on rings A and B is described.

     

Radical addition reactions: factors determining the transition-state geometry

Interatomic distances in the reaction centers of the addition reactions of (i) H^· to the C=C, C=O, N≡C, and C≡C bonds, (ii) ^·CH₃ radical to the C=C, C=O, and C≡C bonds, and (iii) alkyl, aminyl, and alkoxyl radicals to olefin C=C bonds were determined using a new semiempirical method for calculating transition-state geometries of radical reactions. For all reactions of the type X^· + Y=Z → X— Y—Z^· the r ^# _X...Y distance in the transition state is a linear function of the enthalpy of reaction. Parameters of this dependence were determined for seventeen classes of radical addition reactions. The bond elongation, Δr ^# _X...Y, in the transition state decreases as the triplet repulsion, electronegativity difference between the atoms X and Y in the reaction center, and the force constant of the attacked multiple bond increase. __________ Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 894–902, April, 2005.     

芳香酸淋洗液的单柱阳离子色谱法测定碱金属,铵离子和烷基胺

研究了邻苯二甲酸、苯甲酸和对羟基苯甲酸３种芳香酸分别做淋洗液的单柱阳离子色谱法分离测定Ｌｉ＋、Ｎａ＋、ＮＨ４＋、Ｋ＋、甲胺、乙胺和正丙胺７种物质。３种芳香酸做淋洗液均可将７种物质分离开，且分离结果差异不大。在淋洗液浓度相同的条件下，邻苯二甲酸做淋洗液测定的检出限较低。选择３．０ ｍｍｏｌ／Ｌ邻苯二甲酸做淋洗液测得了上述７种物质的检出限和线性范围，并进行了叶面肥试样分析，７种物质的加标回收率在９６．４％～９８．６％之间。     

Synthesis of novel derivatives of 2-(azolylimino)thiazoline

Successive alkylation of 5-(3-phenylthioureido)-3H-imidazole-4-carboxamides with alkyl halides and chloroacetone gave (N-oxopropylimidazolyl)isothioureas, which were easily converted into derivatives of purine and imidazopyrazinone. In the case of ethyl 5-(3-phenylthioureido)-3H-imidazole-4-carboxylate, primary alkylation occurs at the N atom of the imidazole ring. Reactions of 5-(3-phenylthioureido)-3H-imidazole-4-carboxamides with haloketones afforded a number of 4-hydroxy-2-imidazolyliminothiazolidines and 2-imidazolylimino-Δ⁴-thiazolines.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 2196–2204, October, 2004.     

Synthesis of alkyl (α-phenylthioalkenyl) ketones containing a (Z)-trisubstituted olefinic fragment

Warren"s method, which has been proposed for the synthesis of -phenylthiodialkyl ketones, appeared to be inefficient for the preparation of their alkenyl alkyl analogs. The latter were prepared in good yields by alkenylation of alkyl phenylthiomethyl ketones with alkenyl bromides.     

红收获蚁信息素的鉴定

利用色谱－质谱联机技术，在红收获蚁P.barbatus和P.maricopa的毒腺体样品中检测到召引信息素甲基吡嗪（MP）、2，5－二吡嗪（DMP）、3－乙基－2，5－二甲基吡嗪（EDMP）、和三甲基吡嗪（TMP）。利用特征离子色谱技术，在P.barbatus样品中还检测到了含6个碳原子侧链烃基的吡嗪X。根据吡嗪X的质谱图推测其结构为3－仲丁基－2，5－二甲基吡嗪（BDMP）。P.barbatus中DMP，TMP和EDMP的平均相对百分比分别为60.71、26.49、12.80；标准偏差分别为6.91、4.92、5.11;P.maricopa中平均相对百分比和标准偏差分别为47.48、20.35、32.17和15.05、4.05、15.44。