| N-甲基四氢咔唑酮的绿色合成工艺初探 |
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| 引用本文： | 黄倪丽,丁为民,牛古丹.N-甲基四氢咔唑酮的绿色合成工艺初探[J].化学与粘合,2012(2):81-83. |
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| 作者姓名： | 黄倪丽 丁为民 牛古丹 |
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| 作者单位： | [1]黑龙江省科学院石油化学研究院,黑龙江哈尔滨150040 [2]哈尔滨理工大学化学与环境工程学院,黑龙江哈尔滨150080 |
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| 摘 要： | 以N,N-二甲基甲酰胺作溶剂,四丁基溴化铵作相转移催化剂,碳酸二甲酯作甲基化试剂,由四氢咔唑酮与氢氧化钾反应先合成钾盐,再经甲基化合成了N-甲基四氢咔唑酮。考察了钾盐与碳酸二甲酯的配比、反应时间、溶剂用量、催化剂及催化剂用量等因素对反应收率的影响。较佳合成条件为碳酸二甲酯∶四氢咔唑酮钾盐=2.5∶1,四丁基溴化铵用量为钾盐物质的量的2%,在100℃反应10h,反应摩尔收率可达80%以上。
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| 关 键 词： | N-甲基四氢咔唑酮 四氢咔唑酮 碳酸二甲酯 甲基化 |
Study on a Novel Green Synthetic Technology for N-Methy-l,2,3,4-Tetrahydrocarbazole-4-one |
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| HUANG Xian-li,DING Wei-min and NIU Gu-dan.Study on a Novel Green Synthetic Technology for N-Methy-l,2,3,4-Tetrahydrocarbazole-4-one[J].Chemistry and Adhesion,2012(2):81-83. |
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| Authors: | HUANG Xian-li DING Wei-min and NIU Gu-dan |
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| Affiliation: | 1.1nstitute of Petrochemistry, Heilongjiang Academy of Science, Harbin 150040, China;2. College of Chemistry and Environmental Engineering, Harbin University of Science and Technology, Harbin 150080, China) |
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| Abstract: | The intermediate, potassium salt of tetrahydro-carbazol-4-one was synthesized from tetrahydro-carbazol-4-one and KOH at first, in the presence of tetrabutyl ammonium bromide （TBAB） as the phase transfer catalyst （PTC）, N,N-dimethylformamide （DMF） as the solvent, and dimethyl carbonate（DMC）as the methylating reagent. Then N-methy-l,2,3,4-tetrahydrocarbazole-g-one was prepared by methylation of the intermedi- ate. The best yield（~〉80%） of N-methy-l,2,3,4-tetrahydrocarbazole-4-one was obtained under the optimized conditions： n（DMC）：n（tbe intermediate）= 2.5：1, n（TBAB）/n（potassium salt）=2% （molar ratio）, the reaction temperature was 100 °C and the reaction time was 10h. The molar yield of this reac- tion could reach over 80%. |
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| Keywords: | N-Methy-l 2 3 4-tetrahydrocarbazole-4-one tetrahydro-carbazol-4-one dimethyl carbonate methylation |
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