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以甲基磺酰氯为原料,通过氨解反应合成了甲基磺酰胺,探讨了合成反应的工艺条件。实验表明,当原料用量与溶剂的体积比为1:5时,反应温度控制在35-40℃之间,用环己烷作为反应的溶剂,并以乙醇作萃取分离剂,可使产品的收率达87%-89%。 相似文献
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高纯度甲基磺酰胺的合成 总被引:1,自引:0,他引:1
甲基磺酰胺是合成高效除草剂虎威的重要原料,也是药物及其他精细化工产品的重要中间体。关于它的合成国外文献有大量的报道,主要是以甲基磺酰氯通氨的办法生产甲基磺酰胺。文献选择了不同的溶剂进行反应,如用苯[1~4]、甲苯[5]、四氢呋喃、N,N-二甲基甲酰胺... 相似文献
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新型玉米田除草剂甲基磺草酮的合成研究 总被引:6,自引:0,他引:6
以2-硝基-4-甲磺酰基一笨甲酰氯和1,3-环己二酮为原料,首先碱性条件下合成烯醇酯,然后再经催化重排制得甲基磺酮,讨论了反应条件对产品收率的影响并得到了适宜的工艺条件。结果表明,在以二氯甲烷为溶剂,三乙胺为缚酸剂,重排温度为50℃时,所得甲基磺草酮产品含量≥95.0%,收率≥70.0%。 相似文献
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芳磺酰异硫氰酸酯的合成工艺研究 总被引:2,自引:0,他引:2
报道了以芳磺酰胺为起始原料,与氢氧化钾在N,N-二甲基甲酰胺中混合,滴加二硫化碳,在氮气保护下于45°C反应7.5 h,析出棕黄色二硫代芳磺酰亚胺钾盐。过滤,真空干燥,将所得化合物悬浮于无水二氯乙烷中,滴加二(三氯甲基)碳酸酯二氯乙烷溶液,1.5 h加毕,在45°C下持续反应15 h,得芳磺酰异硫氰酸酯,产率61%~75%。 相似文献
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以4-甲基苯磺酰氯和水合肼为原料,甲苯为溶剂合成了对甲基苯磺酰肼。得出的最佳合成条件为:n(4-甲基苯磺酰氯):n(水合肼)=1:1.2,室温反应20min,产品收率为92.0%。 相似文献
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陈湘平 《化学推进剂与高分子材料》2000,(2)
以丙烯酰胺和甲醛为原料,浓盐酸为催化剂,在1,2-二氯乙烷溶剂中于75~80℃下反应2h,合成了N,N′-亚甲基双丙烯酰胺,产率达88.46%,IR谱图与进口纯品一致。讨论了影响合成的各种因素。 相似文献
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T. M. Luong H. Schriftman Daniel Swern 《Journal of the American Oil Chemists' Society》1967,44(5):316-320
The direct preparation ofthreo-1,2-glycols without isolation of intermediates from oleic acid, methyl oleate, and oleyl alcohol by oxidation with a hydrogen
peroxide (70%)-tungstic acid system at pH 0–1 and 45–55C without solvent has now been shown to be an efficient, high-yield
reaction. Thethreo-isomers are formed from intermediate epoxides by in situ hydration with accompanying inversion. Preincorporation of about
2% of the glycol reaction product into oleic acid or methyl oleate speeds up the oxidation reactions markedly and adds to
their control and reproducibility. With oleyl alcohol, addition of reaction product is not necessary.
Castor and olive oils are also readily oxidized to almost complete elimination of unsaturation, but the products are only
50–60% 1,2-glycols, owing to intra- and intermolecular polyether information. Addition of reaction product is unnecessary
with castor oil, but with olive oil the reaction rate is greatly accelerated by incorporation of 2% of reaction product. Preconditioning
(5 hr) of the hydrogen peroxide with the tungstic acid permits slightly faster oxidation rates. Emulsions are also rapidly
oxidized under appropriate conditions, but these systems are more complicated to prepare and work up than oxidation of the
substrates directly. Tentative reaction mechanisms are proposed in which an inorganic polyperoxytungstic acid is the effective
oxidizing agent and hydroxyl-containing species are important interfacial or complexing agents between the substrate and oxidant
system.
Presented in part at the AOCS Meeting in Philadelphia, October 1966.
Present address: Warner-Lambert Research Institute, Morris Plains, N. J. Work completed in partial fulfillment of the requirements
for the PhD degree. 相似文献
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The synthesis of 1,2-disubstituted perhydropyridazine-3,6-diones in high yield is described. The reaction of succinic anhydride and 1,2-dialkylhydrazines leads to N,N′-dialkyl-3-carboxypropionhydrazides which are converted to 1,2-dialkylperhydropyridazine-3,6-diones in refluxing xylene or polyphosphoric acid. The reaction of 1,2-diarylhydrazines with 3-carbomethoxypropionyl chloride and hydrolysis of the resulting N,N′-diaryl-3-carbomethoxypropionhydrazides yields N,N′-diaryl-3-carboxypropionhydrazides. Cyclization of these acid-hydrazides in thionyl chloride at low temperature affords the corresponding 1, 2-diarylperhydropyridazine-3,6-diones. The alkylation of 1,2-dipropyl-perhydropyridazine-3,6-dione in various base-solvent systems with methyl and isopropyl iodide is reported. 相似文献
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Hwee Yoong Felicia Gok Jianhneg Shen Shahram Emami Martin J. T. Reaney 《Journal of the American Oil Chemists' Society》2013,90(2):291-298
A metal methoxide is more expensive than a metal hydroxide and dissolves in methanol releasing a methoxide ion without producing water. The methoxide ion has a higher reaction rate making it more preferred for industrial biodiesel production. This study describes the preparation of alkoxide catalysts from metal hydroxides and non-volatile, non-toxic polyols. Heating aqueous solutions of metal hydroxides and different polyols (1,2-propanediol, 1,3-propanediol, glycerol, xylitol and sorbitol) under vacuum yielded polyol-derived alkoxide base catalysts (PDABC). Comparison of the drying process for respective sodium hydroxide-polyol combinations at two mole ratios of sodium hydroxide to polyol showed that drying at 2:1 mole ratio (metal hydroxide to polyol) was more efficient than that of 3:1. Dehydration of alkaline solutions containing three or more hydroxyl groups (glycerol, sorbitol and xylitol) was faster than drying similar solutions of diols. The empirical formula determined confirmed that the resulting powders contained mono-sodium substituted alkoxides at 1:1, 2:1 and 3:1 (sodium hydroxide: polyol) mole ratio. Fatty acid methyl esters were prepared from canola oil and methanol using glycerol sodium alkylate as a catalyst. The conversion yield of oil to methyl ester was greater than 99 %. 相似文献
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以正丁基锂为引发剂、环己烷/己烷为溶剂,采用间歇聚合工艺模拟溶聚丁苯橡胶(SSBR)聚合过程的凝胶生成实验,考察了1,2-丁二烯的抑凝机理.结果表明:1,2-丁二烯具有明显抑凝作用,加入质量分数为(1~5)×10-5时,产品的凝胶质量分数在0.010%以内;其加入质量分数高于5×10-5时,产品的凝胶质量分数低于0.001%;1,2-丁二烯加入量质量分数超过1×10-4时,对聚合反应速率和单体转化率有影响.1,2-丁二烯作为抑凝剂可有效解决连续聚合SSBR工艺中的凝胶挂堵问题. 相似文献
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二乙醇胺与乙酰乙酸甲酯反应合成了硼酸酯键合剂原料N,N-二羟乙基乙酰乙酰胺。通过均匀设计与SPSS软件处理实验数据,确定了N,N-二羟乙基乙酰乙酰胺收率与各反应因素的回归方程;最佳反应条件为:n(乙酰乙酸甲酯)/n(二乙醇胺)=1.3,催化剂w(ZnAc2.2H2O)=0.25%(以二乙醇胺的质量计,以下同),反应温度140℃,反应时间2.5 h,减压蒸除未反应原料得产物。在该条件下,N,N-二羟乙基乙酰乙酰胺收率达84.9%。以N,N-二羟乙基乙酰乙酰胺制备的硼酸酯键合剂BA-5-2在5 L高能丁羟四组元推进剂装药实验中的应用结果显示:推进剂常温、高温各项力学性能指标均高于发动机设计要求15%,高温黏附指数φ=1.037,其综合力学性能优于醇胺类键合剂LAB-303B、二乙醇胺硼酸酯键合剂BAG-5及海因三嗪类键合剂BA603。 相似文献
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高透明UV稀释剂三羟甲基丙烷三丙烯酸酯的制备研究 总被引:7,自引:1,他引:6
研究了在对甲苯磺酸的催化下,三羟甲基丙烷和丙烯酸在含有阻聚剂在对苯二酚的苯溶剂中反应,经过中和,洗涤,脱溶和真空脱水,得到高透明UV稀释剂三羟甲基丙烷三丙烯酸酯,收率>95%。 相似文献
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