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| Preparation of Tetrahydro-1, 3-dimethyl-2(1H) pyrimidine |
| HUANG Zhi-guo,QU Shu-yu,LIANG Li-ming |
| Cangzhou Shuiyifang Membrane Technology Corporation Ltd.,Cangzhou 061000,China |
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Abstract Tetrahydro-1,3-dimethyl-2(1H) pyrimidine(DMPU) was prepared via cyclization and methylation reactions with 1,3-diaminopropane,urea,polyoxymethylene and formic acid as raw materials.The structure of the product was characterized by IR and 1H NMR,the purity of product was analyzed by gas chromatography,the water content in the product was determined by Karl fischer titration. The influences of solvent, material concentration,material ratio, reaction temperature and reaction time, catalyst on the synthesis process were studied. The best conditions were water-ethylene glycol solution was using as solvent when pyrimidine was prepared;the molar ratio of paraformaldehyde and formic acid was 1:3.75,reaction temperature was 110~120 ℃,reaction time was 16 h,cuprous chloride and triethylamine were selected as catalyst,and their amout was 1.0% of pyrimidine respectively. The yield of DMPU could reach 71% and the purity could reach 98.5%.
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| [ 1 ] 姚转乐,姬明理,王融冰,等. 1,3-二甲基-2-咪唑啉酮的制备[ J ]. 应用化工 2009,38(9):1 83-1 285.[ 2 ] 杨彩宁,樊永惠,刘红妮,等. 1,3-二甲基-2-咪唑啉酮的纯度测定[ M ]. 分析测试技术与仪器 2010,16(4):253 - 256.[ 3 ] 费振荣. 1,3-二甲基-2-咪唑啉酮的合成和应用[ J ]. 上海燃料,2004,32(1):22 - 23.[ 4 ] 韩 斌,尹 宁,毛桂红,等. N, N-二烷基撑基环脲类化合物的合成工艺研究[ J ] . 天津理工大学学报 2011,27(3): 76 - 80.[ 5 ] 张士英,吴达俊,杨悟子. N,N-二甲基-2-咪唑啉酮的合成[ J ]. 化学试剂,1997,19(3):181 - 182.[ 6 ] Fmnz Lothar,Eggersdorfer Manfred.Process for the preparation of cyclic N,N-dimethyl urea[ P ]. DE:3800083,1989-07-13. |
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