| 4,5-二氢-3-甲基-1-(4-氯-2-氟苯基)-4-二氟甲基-1,2,4-三唑-5(1H)酮的合成工艺研究 |
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| 引用本文： | 张新兵,盛文辉,陈海群.4,5-二氢-3-甲基-1-(4-氯-2-氟苯基)-4-二氟甲基-1,2,4-三唑-5(1H)酮的合成工艺研究[J].精细石油化工,2012,29(1):63-65. |
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| 作者姓名： | 张新兵 盛文辉 陈海群 |
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| 作者单位： | 1. 常州大学怀德学院,江苏常州,213016
2. 常州大学江苏省精细化工重点实验室,江苏常州,213164 |
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| 摘 要： | 以4,5-二氢-3-甲基-1-(4-氯-2-氟苯基)-1,2,4-三唑-5(1 H)酮的钾盐为原料,与一氯二氟甲烷进行N-烷基化反应合成了4,5-二氢-3-甲基-1-(4-氯-2-氟苯基)-4-二氟甲基-1,2,4-三唑-5(1 H)酮。研究了不同原料、碱性试剂用量、反应温度等因素对反应收率的影响,实验结果表明,最佳工艺条件为:n(钾盐)∶n(碳酸钾)=1∶2,m(钾盐)∶m(N-甲基吡咯烷酮)=1∶5,反应温度165℃,在此条件下,产物收率≥56%,质量分数≥95%。
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| 关 键 词： | 4 5-二氢-3-甲基-1-(4-氯-2-氟苯基)-4-二氟甲基-1 2 4-三唑-5(1H)酮 钾盐 一氯二氟甲烷 N-烷基化 唑酮草酯 |
SYNTHESIS OF 4,5-DIHYDRO-3-METHYL-1-(4-CHLORO-2-FLUOROPHENYL)-4-DIFLUOROMETHYL-1,2,4-TRIAZOL-5-( 1 H )-ONE |
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| Zhang Xinbing
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Sheng Wenhui
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Chen Haiqun.SYNTHESIS OF 4,5-DIHYDRO-3-METHYL-1-(4-CHLORO-2-FLUOROPHENYL)-4-DIFLUOROMETHYL-1,2,4-TRIAZOL-5-( 1 H )-ONE[J].Speciality Petrochemicals,2012,29(1):63-65. |
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| Authors: | Zhang Xinbing Sheng Wenhui Chen Haiqun |
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| Affiliation: | 1.Huaide Colloge of Changzhou University,Changzhou 213016,Jiangsu,China; 2.Key Laboratory of Fine Chemical Engineering of Changzhou University, Changzhou 213164,Jiangsu,China) |
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| Abstract: | 4,5-Dihydro-3-methyl-1-(4-chloro-2-fluorophenyl)-4-difluoromethyl-1,2,4-triazol-5-(1H)-one was synthesized by the N-alkylation of the potassium salt of 4,5-dihydro-3-methyl-1-(4-chloro-2-fluorophenyl)-1,2,4-triazol-5(1H)-one with chlorodifluoromethane at 165 ℃.The yield of the product was above 56 % and the purity was above 95%.The effect of raw materials,amounts of alkali,reaction temperature on the yield of N-alkylation was investigated.The optimal reaction conditions were found as follows: n(potassium salt)∶n(K2CO3)=1∶2,m(potassium salt)∶m(NMP)=1∶5. |
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| Keywords: | 4 5-dihydro-3-methyl-1-(4-chloro-2-fluorophenyl)-4-difluoromethyl-1 2 4-triazol-5-(1H)-one potassium salt chlorodifluoromethane N-alkylation carfentra-zone-ethyl |
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