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Tebufenpyrad, a new high effective pyrazoleamide acaricide , was synthesized from 1-methyl-3-ethyl-4-chloro-5-pyrazolecarbon acid and 4-t-butylbenzylamine, the raw material are propionyl pyruvic ethyl ester and 4-t-butyl benzylchloride.

吡螨胺是一种新型、高效的吡唑酰胺类杀螨剂,本文以中间体1-甲基-3-乙基-4-氯-5-吡唑甲酸和4-叔丁基苄胺合成,起始原料丙酰丙酮酸乙酯和4-叔丁基苄氯,总收率为61.23%。

Methods 4-Hydroxy- benzonitrile was treated with sodium hydrogen sulfide and anhydrous magnesium chloride in dimethyl formamide to give thioamide, which was then directly cyclized with ethyl 2-chloroacetoacetate without separation to give ethyl 2-(4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(2) in one-pot; then 2 was formylated with Duff reaction adopting hexamethylenetetramine in trifluoroacetic acid to give ethyl 2-(3-formyl-4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(3); finally, the target compound was obtained by the treatment of 3 with hydroxylamine hydrochloride and sodium formate in formic acid.

采用"一勺烩"方法,以4-羟基苯甲腈为起始原料,首先与硫氢化钠和无水氯化镁在N,N-二甲基甲酰胺中反应,所得中间体不经分离,直接加入2-氯乙酰乙酸乙酯进行环合反应,得到2-(4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯(2);然后通过六亚甲基四胺/三氟乙酸进行Duff反应,得到2-(3-甲酰基-4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯(3);再经盐酸羟胺/甲酸/甲酸钠体系脱水得到目标化合物。

Mainly engaged in: Hydrogen-imide hydrochloride, o-chlorophenyl cyclopentanone, 3.4 dimethoxy ethyl benzene, butyn single potassium acid, potassium ethyl malonyl, Ding amide, amide isobutyraldehyde , allyl chloroacetate, isopropyl chloroacetate Benzyl aluminum, cyclopentene, cyanide-o-chlorophenyl, o-methyl chloride, sulfuric acid chloride, p-chlorophenol, imidazole, Pinacolone, one chlorine Pinacolone.

主要经营:盐酸氢亚胺、邻氯苯基环戊酮、3.4二甲氧基苯乙酯、丁炔二酸单钾盐、丙二酸单乙酯钾盐、丁酰胺、异丁酰胺、氯乙酸烯丙酯、氯乙酸苄酯异丙醇铝、环戊烯、邻氯苯氰、邻氯苯甲酯氯、硫酸氯、对氯苯酚、咪唑、频呐酮、一氯频呐酮。

Both the protection and deprotective group methods for the amino-group on side chain of a new N-pivot lariat crown ether were studied comparatively.

研究了一种新的氮支套素冠醚侧链上氨基的保护和脱保护基方法,结果表明,由过量乙二胺与对甲苯磺酰氯反应得到的单保护乙二胺(N-对甲苯磺酰基乙二胺4a),经N-烷基化环化反应,然后在氢化铝锂存在下脱除保护基,即可制得最佳产率的N-(2-氨基已基)单氮杂-12-冠-4(1)。

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%。

The results show that:(1) When N-methylethylenediamine and N, N'-methylethylenediamine equatorially coordinated to Cd〓, arenedisulfonates such as 1, 5-naphthalenedisulfonate, 2, 6-naphthalenedisulfonate and 4, 4'-bipenyldisulfonate act as a bridging ligands coordinated to adjacent Cd〓 centers, leading to a one dimensional chain structure.

研究结果表明:(1)N-甲基乙二胺和N,N'-二甲基乙二胺与Cd〓在赤道平面配位后,芳烃二磺酸根离子作为桥联配体与相邻的Cd〓在轴向配位形成了一维链状结构。

The invention relates to a synthesis method of N-acetylaminoglucose, which comprises dissolving D-glucosamine hydrochlorate and alcohol at the mass ratio of 2-2.5:100, adjusting the pH value of the solution to 9-10, filtering, taking the filter liquor, mixing and adding acetic anhydride at the 50-60wt% amount of D-glucosamine hydrochlorate, mixing and reacting for 2h, using absolute ethyl alcohol to recrystallizing, filtering and recrystallizing via water, to obtain rod-shape food grade N-acetylaminoglucose.

本发明涉及一种N-乙酰氨基葡萄糖的合成方法。该方法的具体步骤为:将D-葡萄糖胺盐酸盐和乙醇按2~2.5∶100的质量比溶于水中,调节该溶液的pH值为9~10;过滤,取滤液,搅拌下加入乙酸酐,其加入量为原料D-葡萄糖胺盐酸盐量的50~60wt%;搅拌反应2小时后,用无水乙醇进行重结晶;过滤,晶体再用水重结晶,得棒状食品级N-乙酰氨基葡萄糖。

Methods 4-Hydroxy- benzonitrile was treated with sodium hydrogen sulfide and anhydrous magnesium chloride in dimethyl formamide to give thioamide, which was then directly cyclized with ethyl 2-chloroacetoacetate without separation to give ethyl 2-(4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(2) in one-pot; then 2 was formylated with Duff reaction adopting hexamethylenetetramine in trifluoroacetic acid to give ethyl 2-(3-formyl-4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(3); finally, the target compound was obtained by the treatment of 3 with hydroxylamine hydrochloride and sodium formate in formic acid.

采用&一勺烩&方法,以4-羟基苯甲腈为起始原料,首先与硫氢化钠和无水氯化镁在N,N-二甲基甲酰胺中反应,所得中间体不经分离,直接加入2-氯乙酰乙酸乙酯进行环合反应,得到2-(4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯(2);然后通过六亚甲基四胺/三氟乙酸进行Duff反应,得到2-(3-甲酰基-4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯(3);再经盐酸羟胺/甲酸/甲酸钠体系脱水得到目标化合物。

To study the relationship between the hydrophobic "tail" structure and thecharacterizations of Gemini surfactants, a new gemini surfactant CsH2s-α,ω-bis(dehydroabietylhydroxypropylteteramethylethylammonium Chloride),here s=2, wassynthesized. Dehydrogenated rosin as hydrophobic "tails" in the structure. The impact factorsin the two steps are discussed.

为研究gemini表面活性剂中疏水&尾巴&结构对性质的影响,本论文以脱氢松香酸和环氧氯丙烷为原料合成了中间体3-脱氢松香酰氧-2-羟丙基氯,再与四甲基乙二胺反应,得到一种以脱氢松香酰基为疏水链&尾巴&的对称gemini型双季铵盐阳离子表面活性剂:二氯化-N,N′-二(3-脱氢松香酰氧-2-羟丙基)四甲基乙二胺。

A plausible process of this reaction is as following: Aldehyde was in equilibrium with the enol form, aldehyde reacted with aniline catalyzed by 2,2,2-trichloroacetic acid to afford imine, the generated imine immediately reacted with enol to form intermediate via intramolecular cyclization.

我们发现一分子芳基叠氮和一分子三苯基磷反应生成一分子磷亚胺,后者与由两分子取代的苯氧乙酰氯原位生成的烯酮反应生成4-亚烷基-β-烷基-内酰胺,其串联过程涉及烯酮亚胺的形成及其与烯酮的[2+2]的环加成反应。

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