N-甲基四氢咔唑酮的绿色合成工艺初探

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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。 Using N, N-dimethylformamide as a solvent, tetrabutylammonium bromide as a phase transfer catalyst and dimethyl carbonate as a methylation reagent, and reacting the tetrahydrocarbazolone with potassium hydroxide to synthesize a potassium salt first, N-methyl tetrahydrocarbazolone was synthesized by methylation. The effects of the ratio of potassium salt to dimethyl carbonate, the reaction time, the amount of solvent, the amount of catalyst and catalyst on the reaction yield were investigated. The optimum synthesis conditions are as follows: dimethyl carbonate: potassium tetrahydrocarbazone = 2.5: 1, tetrabutylammonium bromide is 2% of the amount of potassium salt and reacted at 100 ℃ for 10h. The molar yield of the reaction can be Up to 80%.
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