Condensation of secondary amines with CH-acids and formaldehyde under the influence of microwave radiation

A. I. Musin, D. S. Sultanova, Y. Borisova, T. P. Mudrik, R. Daminev
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Abstract

Objectives. To synthesize tertiary amines containing gem-dichlorocyclopropane or 1,3-dioxolane fragmentusing the Mannich reaction, as well as obtain ethyl ester of β-aminopropionic acidbydecarboxylation of tert-amine, a derivative of diethylmalonate containing a gem- dichlorocyclopropane fragment.Methods. In order to obtain tertiary amines by the Mannich reaction, the microwave activation method was used. To determine the qualitative and quantitative composition of the reaction masses, gas chromatography, electron ionization mass spectrometry, and 1H-, 13C-nuclear magnetic resonance spectrometry methodswere used.Results. Under microwave radiationconditions, tertiary amines containing gem- dichlorocyclopropane or 1,3-dioxolane fragment were synthesized by condensation of secondary amines, CH-acids, and paraformaldehyde.Conclusions. Tertiary amines containing a gem-dichlorocyclopropane or cycloacetal fragment in their structure were obtainedin high yields under microwave radiation.
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微波辐射影响下仲胺与ch酸及甲醛的缩合反应
目标。采用曼尼希反应合成含宝石-二氯环丙烷片段或1,3-二氧环烷片段的叔胺,以及含宝石-二氯环丙烷片段的丙二酸二乙酯衍生物叔胺脱羧制得β-氨基丙酸乙酯。为了用曼尼希反应得到叔胺,采用微波活化法。采用气相色谱法、电子电离质谱法、1H-、13c核磁共振谱法测定反应质量的定性和定量组成。在微波辐射条件下,由仲胺、ch -酸和多聚甲醛缩合合成了含宝石-二氯环丙烷或1,3-二氧环烷片段的叔胺。在微波辐射下,以高收率制备了结构上含有宝石-二氯环丙烷或环缩醛片段的叔胺。
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