乙二酰胺

In this paper, acetanilide used as start material was chlorosulfonated, then reacted with alkylamines with different length of carbon chain to prepare 4 p-acetylaminophenylsulfonylalkylamine.

本文以乙酰苯胺为起始原料，经氯磺化后分别和不同碳链的正烷基胺反应制得4种不同碳链长度的对乙酰氨基苯磺酰烷基胺，将其水解后制得了对氨基苯磺酰正丁胺、对氨基苯磺酰正辛胺、对氨基苯磺酰正十二胺和对氨基苯磺酰正十八胺。

We have had the extensive studies on theα-acetyl-α-carbamoyl ketene--acetals and its further applications, for example, their adols condensations with aldehydes giveα-alkenoyl-α-carbamoyl ketene--acetals which can be utilized as the 1,5-bielectronic five-carbon components to react with various binucleophlilic species in a [5+1] annulation.

我们小组在以前的工作中对α-乙酰基-α-胺甲酰基二硫缩烯酮在合成中的应用进行了深入的研究，如与醛缩合生成α-烯酰基-α-胺甲酰基二硫缩烯酮，将其作为1，5-双亲电五碳合成子的[5+1]成环策略等。

In our research on study chemical reaction of active methylene compounds and brom-acetophenone. Because of brom-acetophenone is compound that contain carbonyl and halogen ,which will take place electrophilic substitution and nucleophilic addition. When active methylene compounds are ethyl acetoacetate and β-diketone, controlling reaction condition, we have found that mono-substitution's production and di-substitution's. production is isolated; active methylene compounds are acetoacetanilide and acetoacetanilide derivate, pyrrolidin-2-one derivants were obtained by substitution and close-ring reaction .but there is no report about it.

本文是让活泼亚甲基类化合物与溴代苯乙酮发生化学反应，由于溴代苯乙酮是含有羰基的卤代烃结构，它可以发生亲电取代和亲核加成反应，当活泼亚甲基类化合物为乙酰乙酸乙酯和β-二酮时，控制反应条件可以发生单取代和双取代两种产物；当活泼亚甲基类化合物为乙酰乙酰芳胺类化合物来反应时，溴代苯乙酮中的羰基与氨基会发生分子内的关环反应生成吡咯烷-2-酮衍生物，这在以前的研究中是没有发现的。

When the catalyst was triethylamine, the water produced in condensation of isopropanolamine or ethanolamine and butanone was removed with benzene by water segregator, then the dichloroacetyl chloride was dropped.

利用异丙醇胺、乙醇胺、丁酮和二氯乙酰氯为原料，分别合成了两种除草剂安全剂Ⅰ∶3-二氯乙酰基-2，5-二甲基-2-乙基-1，3-噁唑烷和Ⅱ∶3-二氯乙酰基-2-甲基-2-乙基-1，3-噁唑烷。

Firstly, 3-ethylthiobutanal was prepared from crotonaldehyde reacting with ethanehiol in triethylamine with high yield. Secondly, methyl acetoacetate was converted to 6-ethylthiohept-3-en-2-one by three steps via hydrolysis, condensation with 3-ethyltio-butanal and dehydration, then 6-ethylthiohept-3-en-2-one was cycloco ndensed with dimethyl malonate by Michael addition and Claisen condensation, followed by saponification and decarboxylation to give the intermediate of 5-(2-ethylthiopropyl)-cyclohexane-1,3-dione.

首先，以巴豆醛与乙硫醇为原料，在三乙胺的催化作用下高收率制得3-乙硫基丁醛；然后从乙酰乙酸甲酯出发，通过碱水解、与3-乙硫基丁醛缩合、脱水三步反应合成6-乙硫基-3-烯-2-庚酮，接着6-乙硫基-3-烯-2-庚酮与丙二酸二甲酯通过Michael加成和Claisen缩合成环，再通过皂化和脱羧反应生成中间体5-[2-丙基]-1，3-环己二酮；再与丙酸酐反应丙酰化，最后与0-3-氯-2-丙烯基羟胺肟化，得到目标化合物烯草酮。

Synthesis of Antidote of N-Dichloroacetyl-2-methyl-1-oxa-4-aza-spiro-4.4-nonane BI Hong-mei, ZHANG Jin-yan, LIANG Ying, SHEN Yong (College of Arts and Sciences Heilongjiang August First Reclamation University, Daqing 163319, Heilongjiang, China) Abstract: N-Dichloroacetyl-2-methyl-1-oxa-4-aza-spiro-4.4-nonane was synthesized by one pot method with isopropanolamine, cyclopentanone and dichloroacetyl chloride. The optimum reaction conditions obtained are as follows:the proportion in moles of the above materials is 1∶1∶1.2, reaction solvent is toluene, reaction temperature is -15 to -10 ℃,reaction time is 3 h, under the optimum condition, the yield of the compound is 50.0%.

除草剂解毒剂N-二氯乙酰基-2-甲基-1-氧杂-4-氮杂-螺[4.4]壬烷的合成毕洪梅，张金艳，梁英，沈勇(黑龙江八一农垦大学文理学院，黑龙江大庆 163319)摘要：以33%的氢氧化钠水溶液为缚酸剂，异丙醇胺、环戊酮和二氯乙酰氯为原料，采用&一锅法&合成了N-二氯乙酰基-2-甲基-1-氧杂-4-氮杂-螺[4.4]壬烷，采用正交实验法得到最佳反应条件：反应原料摩尔比为1∶1∶1.2，苯作溶剂，反应的温度为-15 ℃~-10 ℃，搅拌时间为3 h，产率达到50.0%。

In the third chapter, the synthesis of5-[(1"S)-1",2"-diacetyl-oxyethyl]-1-phenylpyrazol-3-carboxaldehyde oxime(2) from5-[(1"S)-1",2"-diacetyl-oxyethyl]-1-phenylpyrazol-3-carboxaldehyde(1) and phenyl-hydrazine were introduced firstly. The synthesis of nine dioxapyrrolino[3,4-c]pyrazoles containing chiral pyrazolyl moiety(6a-i) from 2 with N-substituted-phenylmaleimide by nonmetal oxidant IBD-initiated intermolecular 1,3-dipolarcycloaddition was described in detail.

第三章首先以5-[(1′S)-1′，2′-二乙酰氧基乙基]-1-苯基吡唑-3-醛(1)和苯肼为原料，合成了化合物5-(1′S)-1′，2′-二乙酰氧基乙基1-1-苯基吡唑-3-醛-苯腙(2)；再用化合物(2)与N-取代苯基马来酰亚胺反应，利用无金属氧化剂—IBD引发1，3-偶极反应，发生分子间的环加成，合成了9种新型手性吡唑连二氧代吡咯啉并

Three methods for the preparation of 1,2,4-trizolone~5 are provided. 22 compounds are prepared. 3, 4-disubstituted 1,2,4-trizolone-5 is prepared by reacting amide with ethyl hydrazine-fornate at 110癈 for 3h in the presence of phosphorus oxychloride, following neutralization and cyclization reaction, giving to 74.5 % yields,which is 30% more than the literature value.

以三氯氧磷为缩合剂，使酰胺和肼基甲酸乙酯在110℃反应3h，经碱中和、环化反应，合成3，4-二取代-1，2，4-三唑酮-5，两步反应总产率达74.5％，与文献报道值相比，高出了30％以上，在三唑酮类衍生物的合成方法中具有很大的突破性。

X 6.36(3)? is formed.Liquid-liquid extraction experiments, between twelve heterocyclic thioalkoxycalix[4]arene on the lower rim, fifteen heterocyclic thioacetamidecalix[4]arene on the upper rim and Na~+、K~+、Cs~+、Mg~(2+)、Cu~(2+)、Co~(2+)、Cd~(2+)、Ni~(2+)、Pb~(2+)、Hg~(2+) and Ag~+ picrates, have been carried out and their results are compared.

分别将十二个下沿含有杂环硫烷氧基杯芳烃衍生物和十五个上沿含有杂环硫乙酰胺基的杯芳烃衍生物与Na~+、K~+、Cs~+、Mg~(2+)、Cu~(2+)、Co~(2+)、Cd~(2+)、Ni~(2+)、Pb~(2+)、Hg~(2+)和Ag~+的十一种苦味酸盐进行了离子萃取实验，并对两类衍生物与不用金属离子的萃取能力进行了分析和比较。

SiO2 aerogel was prepared by using waterglass as the Si source, formamide as the catalyst and glycol as the drying chemical controlling additive via sol-gel method and ambient pressure drying.

以水玻璃为硅源，甲酰胺为催化剂，乙二醇为干燥控制化学添加剂，采用溶胶－凝胶法常压下干燥制备了硅石气凝胶粉体。

And Pharaoh spoke to Joseph, saying, Your father and your brothers have come to you.

47：5 法老对约瑟说，你父亲和你弟兄们到你这里来了。

Additionally, the approximate flattening of surface strip using lines linking midpoints on perpendicular lines between geodesic curves and the unconditional extreme value method are discussed.

提出了用测地线方程、曲面上两点间短程线来计算膜结构曲面测地线的方法，同时，采用测地线间垂线的中点连线和用无约束极值法进行空间条状曲面近似展开的分析。