湖南师范大学自然科学学报
湖南師範大學自然科學學報
호남사범대학자연과학학보
ACTA SCIENTIARUM NATURALIUM UNIVERSITATIS NORMALIS HUNANENSIS
2009年
4期
77-79
,共3页
2%3%5-三甲基吡嗪%丁二酮%1%2-丙二胺%脱氢芳构化
2%3%5-三甲基吡嗪%丁二酮%1%2-丙二胺%脫氫芳構化
2%3%5-삼갑기필진%정이동%1%2-병이알%탈경방구화
2,3,5-trimethylpyrazine%biacetyl%1,2-diaminopropane%dehydroaromatization
介绍以丁二酮和1,2-丙二胺为原料,经缩合、脱氢芳构化反应合成2,3,5-三甲基吡嗪的新方法.重点考察了脱氢剂组成、脱氢剂用量、溶剂用量等对反应的影响.确定了合成2,3,5-三甲基吡嗪的优化条件为:以无水乙醇为溶剂,投料比为丁二酮:丙二胺:脱氢剂:无水乙醇=1:0.67:1.4:1.31(质量比);缩合反应温度为20～25℃:回流脱氢4 h,2,3,5-三甲基吡嗪的含量达98%以上.
介紹以丁二酮和1,2-丙二胺為原料,經縮閤、脫氫芳構化反應閤成2,3,5-三甲基吡嗪的新方法.重點攷察瞭脫氫劑組成、脫氫劑用量、溶劑用量等對反應的影響.確定瞭閤成2,3,5-三甲基吡嗪的優化條件為:以無水乙醇為溶劑,投料比為丁二酮:丙二胺:脫氫劑:無水乙醇=1:0.67:1.4:1.31(質量比);縮閤反應溫度為20～25℃:迴流脫氫4 h,2,3,5-三甲基吡嗪的含量達98%以上.
개소이정이동화1,2-병이알위원료,경축합、탈경방구화반응합성2,3,5-삼갑기필진적신방법.중점고찰료탈경제조성、탈경제용량、용제용량등대반응적영향.학정료합성2,3,5-삼갑기필진적우화조건위:이무수을순위용제,투료비위정이동:병이알:탈경제:무수을순=1:0.67:1.4:1.31(질량비);축합반응온도위20～25℃:회류탈경4 h,2,3,5-삼갑기필진적함량체98%이상.
A novel method introduce to synthesis 2,3,5-trimethylpyrazine by consendation of biacetyl and 1,2-diaminopropane followed by dehydroarmatization was studied.The composition of dehydrogenation oxidizer.the amount of dehydrogenation oxidizer and solvent were investigated emphatically.The optimum conditions were established as follow:anhydrous ethyl alcohol as solvent,the ratio of biacetyl,1,2-diaminopropane,dehydrogenation oxidizer and solvent is 1:0.67:1.4:1.31(by weight),condensation at 20～25℃,and dehydrogenation at refluxing temperature of ethyl alcohol for 4 h,2,3,5-trimethylpyrazine can be obtained with 98%purity.
