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With trimethyl,4-dodecylbenezyl ammonium chloride and 18-crown-6 as pase-transfer catalysts, the azidation of polyepichlorohydrin in poly and H2O were studied. The reaction discipline and mechanism were discussed. The results show that the system with trimethyl, 4-dodecylbenezyl ammonium chloride as phase transfer catalyst and PEG as medium is a safe and effective approach to glycidyl azide polymer preparation, and azidational ratio of PECH can reach 97% above within 15 h.

研究了氯化十二烷基苄基三甲基铵和18-冠-6为相转移催化剂时端羟基聚环氧氯丙烷在聚环氧乙烷和水为介质中的叠氮化反应,探讨了反应规律和反应机理,结果表明:以PECH为介质,十二烷基苄基三甲基氯化铵(TMDA-1)为相转移催化剂的反应体系,可在15h内使PECH叠氮化转化率达到97%以上,无主链断裂等副反应,是一条较为安全快速的制备叠氮粘合剂的方法。

In this paper, varied factors which influenced the synthesis of epoxypropyl trimethyl ammonium chloride by the reaction of epichlorlhydrin with trimethylamine were studied.

研究了由环氧氮丙烷与三甲胺反应合成环氧丙基三甲基氮化铵沥青乳化剂中间体的各种影响因素。

The 6- cyano-1, 1 (1, 3- dioxypropylidene)-7-(carbomethoxyl group- methyl - 5- oxo-Delt6 (8)- tetrahydrochysene indolizine and haloethane reacts with each other for ethylization with existence of alkali and organic solution with or without phase transversion catalyst, and produces mentioned product.

本发明在相转移催化剂或无相转移催化剂存在下,6-氰基-1,1-(1,3-亚丙二氧基)-7-(甲氧羰基-甲基-5-氧代-Δ6(8)-四氢中氮茚类化合物与卤代乙烷在碱和有机溶剂的存在下进行乙基化反应即得6-氰基-1,1-(1,3-亚丙二氧基)-7-1′-(烷氧羰基-丙基-5-氧代-Δ6(8)-四氢中氮茚类化合物。

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%。

Using butanediol as initiator, boron-trifluoride etherate as catalyst, 3-azidomethyl-3-methyloxetane homopolymer was synthesized by the cationic polymerization of 3-azidomethyl-3-methyloxetane which was carried out in dichlorometane.

以1,4-丁二醇为引发剂,以三氟化硼乙醚络合物为催化剂,以3-叠氮甲基-3-甲基氧丁环为单体,以CH2Cl2为溶剂,按阳离子开环聚合机理,合成了含能粘合剂3-叠氮甲基-3-甲基氧丁环均聚物。

Using pentaerythritol as initiator, boron trifluoride diethyl etherate as catalyst.dichloroethane as dispersion agent, the chloride polyether polyol is synthesized based on the mechanism of cationic ring-opening polymerization of epiclilnrohyclrin.The azide polyether polyol is synthesized, in DMF through A and sodium azide, and the non-reported azide energetic curing agent is synthesized through the adduction of B and IIDI.

以季戊四醇为起始剂,三氟化硼乙醚为催化剂,1,2—二氯乙烷为分散剂,环氧氯丙烷经阳离子开环聚合反应制成氯化聚醚多元醇,A在N,N—二甲基甲酰胺中与叠氮化钠反应制得叠氮聚醚多元醇,B与六亚甲基二异氰酸酯加成反应制得未见文献报道的叠氮固化剂。

The thermal behaviors of CL-20 mixed with three binders (NC+NC, PET and PBT at 160-200℃ were investigated by NBK LAWA gasometric measuring system. The thermal behaviors were described from the changes of evolved gases and decomposition kinetics. Results show that the apparent activation energies of CL-20 and its mixed systems with, PET and PBT are 176.68, 176.31, 136.12 and 127.0 kJmol^(-1), respectively.

用NBK型&拉瓦&量气测试系统研究了较高温度(160~200℃)下六硝基六氮杂异伍兹烷(CL-20)与硝化棉和硝化甘油双基吸收药、环氧乙烷与四氢呋喃共聚醚、3,3-双叠氮甲基氧杂环丁烷与四氢呋喃共聚物三种黏合剂的全分解过程,从放气规律和动力学的变化阐述了CL-20及其与三种黏合剂混合体系的热行为。

In the presence of catalytic rhodium acetate, ethyl 2-diazo-3-oxo-per fluoroalkanoates, reacted readily with nitriles to give a series of 5-fluoroalkyl substituted 1, 3oxazoles with high regio-selectivity through a metal carbenoid intermediate. The reactions of carbenoids with noncyclic vinyl ethers or cyclic vinyl ethers afforded dihydrofuroates in good to excellent yields. Interestingly, only vinyl C-H insertion compound was obtained concerning of the reaction of carbenoids with 2, 5dimethylfuran due to the steric hindrance of methyl group

醋酸铑分解2-重氮-3-氧代-全氟羧酸乙酯形成的金属卡宾作为1,3-偶极体,可以与一系列芳基或烷基取代的腈反应,高度区域选择性地生成一系列4-乙氧羰基-5-氟烷基取代的噁唑化合物;也可以与富电子的链状和环状的烯基醚反应,以优良的产率得到一系列氟烷基取代的二氢呋喃类化合物;而与2,5-二甲基呋喃的反应,由于甲基的位阻作用,只得到金属卡宾对呋喃3-位烯基碳氢键插入产物。

Two types of P Br N contained flame retardant,O (2,4,6 1 trioxo 1 oxyphosphabiscyclooctane 4 methylene) O (2,3 dibromopropyl)phosphoric melamine salt and O (2,4,6 tribromophenyl)phosphoric melamine salt,were synthesized from phosphorus oxychloride,pentaerythritol,2,3 dibromopropanol,2,4,6 tribromophenol and melamine,etc.

以三氯氧磷、季戊四醇、2 ,3 二溴丙醇、2 ,4,6 三溴苯酚及三聚氰胺等为原料合成了两种含磷溴氮阻燃剂,即O (2 ,4,6 三氧杂 1 氧基磷杂双环 [2 。2 。2 ]辛烷 4 亚甲基) O 2 ,3磷酸三聚氰胺盐和O (2 ,4,6 三溴苯基)磷酸三聚氰胺盐。

By further comparing the retention time of the profounds and that of the impurities,the main impurities in triadimefon technical was conformed as following:First, 1-(4-bromophenoxy)-3,3-dimethyl-1 -(1H-1,2,4-triazol-1 -yl)-2-butanone;Second, 1-(2,4-dichlorophenoxy)-3,3-dimethyl-1 -(1H-1,2,4-triazol-1 -yl)-2-butanone;Third, 1,1 -bis(4-chlorophenoxy)-3,3 -dimethy 1-2-butanoneour conclusion is conformed right.

再经过化合物的保留时间与杂质保留时间的比照,证实了三唑酮原药中的主要杂质是:杂质Ⅰ:1-(4-溴苯氧基)-3,3-二甲基-1-(1H-1,2,4-三氮唑-1-基)-2-丁酮;杂质Ⅱ:1-(2,4-二氯苯氧基)-3,3-二甲基-1-(1H-1,2,4-三氮唑-1-基)-2-丁酮;杂质Ⅲ:1,1-二(4-氯苯氧基)-3,3-二甲基-2-丁酮。

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