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二乙酰基胺

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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 this thesis, a convenient and efficient synthesis of highly functionalizeddihydropyrido[2,3-d]pyrimidines via a double [5 + 1] annulation strategy startingfrom easily available α-alkenoyl-α-carbamoyl ketene--acetals 1 and cheapreagents (NH4OAc, DMF, and POCl3) has been developed.

本论文探索了一种简便有效的合成高度官能化的二氢吡啶并[2,3-d]嘧啶的方法,此方法由易得的α-乙酰基-α-氨基乙酰基二硫缩烯酮1和便宜的试剂(醋酸铵,二甲基甲酰胺和三氯氧磷)通过两步[5 + 1]加成而实现。

Through using Mythylene DinitrAmine as rude product, the knowledge of its reaction properties in different phases have been increased, Through using Mythylene BisAcetAmide as rude product, intermediates which include 1,3-Diacetyl -4,5-dihydroxy -1,3-diazacyclopentane and 1,3-Diacetyl- 4,5-diacetoxy-l,3-diaza cyclopentane have been obtained. 2,4,6,8-tetracetyl- 2,4,6,8-tetraaza bicyclo[3,3,0]octane which can be used to produce Bicyclo-HMX by nitrolysis was also produced. Through using Mythylene BisFormAmide as rude product, intermediates which include 1,3-Diformyl-4,5-dihydroxy- 1,3-diazacyclopentane and 1,3-Diformyl- 4,5-diacetoxy-l,3-diazacyclopentane have been abtained.

以亚甲基二硝胺为初始原料,加深了对亚甲基二硝胺在不同反应相反应特征的认识;以亚甲基二乙酰胺为初始原料,制备了中间体1,3-二乙酰基-4,5-二羟基-1,3-二氮杂环戊烷和1,3-二乙酰基-4,5-二乙酰氧基-1,3-二氮杂环戊烷,最终制备了可被直接硝解为双环HMX的2,4,6,8-四乙酰基-2,4,6,8-四氮杂双环[3,3,0]辛烷;以亚甲基二甲酰胺为初始原料,制备了中间体1,3-二甲酰基-4,5-二羟基-1,3-二氮杂环戊烷和1,3-二甲酰基-4,5-二乙酰氧基-1,3-二氮杂环戊烷。

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。

They are 4-(2- hydroxy-3-butynlenoxy) benzoic acid (1, WA), 5-chloro-7, 8-dihydroxy-7-methyl- 6-oxo-3- [ -3, 4-dihydroxy-3, 5-dimethyl-l-heptylene] -1H-8, 8a-dihydrobenzo [2, 3-c] pyran (2, WB),-2-(2-methyl-2-dibutene diamido)-2-butenoic acid (3, B5262), 3, 4-dihydro-9, 10-dihydroxy-7-methoxy-3-methyl-1H-naphtho [2, 3- c] pyran-1-one (4, A73 semi-Vioxanthin), 8, 8'-bis (6, 9-dioxo-3,4-dihydro-10- hydroxy-7-methoxy-3-methyl-1H-naphtho [2, 3-c] pyran-1-one)(5, A122 Xanthomegnin), 2, 5-dioxo-3a-hydroxymethyl-3, 3a, 6, 6a-tetrahydro-furo [2, 3-b] furan (6, 1003-2), 7-acety1-5-chloro-6, 8-dioxo-7-methyl-3- [ -3, 5-dimethyl-1, 3- diheptylene] -4aH-benzo [2, 3-c] pyran (7, M2-2 sclerotiorin), respectively.

它们分别被命名为4-(2-羟基-3-丁炔氧基)苯甲酸(1,WA)、5-氯-7,8-二羟基-7-甲基-6-氧代-3-[-3,4-二羟基-3,5-二甲基-1-庚烯基]-1H-8,8a-二氢苯并[2,3-c]吡喃(2,WB)、-2-(2-甲基-2-丁烯二酰亚胺基)-2-丁烯酸(3,B5262)、3,4-氢-9,10-二羟基-7-甲氧基-3-甲基-1H-萘并[2,3-c]吡喃-1-酮(semi-Vioxanthin,4,A73)、8,8'-双(6,9-二氧代-3,4-二氢-10-羟基-7-甲氧基-3-甲基-1H-萘并[2,3-c]吡喃-1-酮)(Xanthomegnin,5,A122)、2,5-二氧代-3a-羟甲基-3,3a,6,6a-四氢-呋喃并[2,3-b]呋喃(6,1003-2),7-乙酰基-5-氯-6,8-二氧代-7-甲基-3-[-3,5-二甲基-1,3-庚二烯基]-4aH-苯并2,3-c]吡喃(Sclerotiorin,7,M2-2)。

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。

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%。

Experiments show the maximum absorption wavelength of 1,1 diactyl ferrocene and 1,1 DiN, N glucosan...

测定了 1 ,1 -二乙酰基二茂铁、葡胺糖丙酰二茂铁的最大吸收波长,分别是 45 6nm和 346nm。

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

The results showed 3 types of aluminum compound prepared in this paper all had good poison protection effectiveness on such impurities as stannous chloride,lead oxide,sodium hydrogen sulfate,and so on.Moreover,the mechanism of the poison of catalyst was also discussed.

结果表明,合成的3种防中毒剂即防-1、防-2(主要成分为乙酰丙酮合铝)及防-3(主要成分为二乙酰丙酮基异丙氧基铝)对二月桂酸二丁基锡、氯化亚锡、二正丁胺、硫脲、氧化铅及硫酸氢钠等杂质均有较好的防中毒作用;不同防中毒剂对不同杂质的防中毒作用有一定的选择性。

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