| 4-甲基-5-乙氧基噁唑合成工艺研究 |
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| 引用本文： | 杭德余,陈邦和,连祥珍,黄玉兴.4-甲基-5-乙氧基噁唑合成工艺研究[J].精细化工,2002,19(3). |
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| 作者姓名： | 杭德余 陈邦和 连祥珍 黄玉兴 |
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| 作者单位： | 1. 安徽大学化学化工学院,安徽,合肥,230039
2. 清华大学化学系,北京,100084 |
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| 摘 要： | 采用N 乙氧草酰丙氨酸乙酯经环合、水解、酸析和脱羧合成维生素B6的重要中间体 4 甲基 5 乙氧基口恶唑。选用三氯氧磷 /三乙胺 /甲苯 /二甲基甲酰胺作为环合脱水剂 ,当n(N 乙氧草酰丙氨酸乙酯 )∶n(三氯氧磷 )∶n(三乙胺 ) =1 0∶(1 0～ 1 2 )∶(3 5～ 4 2 )时 ,80℃下反应 8h ,环合反应收率为 91 7% ;水解、酸析和脱羧三步一锅 ,收率为 88.2 %。每步产品均运用IR、NMR谱图验证了产品结构
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| 关 键 词： | 维生素B6 4-甲基-5-乙氧基口恶唑 4-甲基-5-乙氧基-2-口恶唑羧酸乙酯 |
Study of the Synthetic Process of 4-Methyl-5-ethoxyoxazole |
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| HANG De yu ,Chen Bang he ,Lian Xiang zhen ,Huang Yu xing.Study of the Synthetic Process of 4-Methyl-5-ethoxyoxazole[J].Fine Chemicals,2002,19(3). |
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| Authors: | HANG De yu Chen Bang he Lian Xiang zhen Huang Yu xing |
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| Affiliation: | HANG De yu 1,Chen Bang he 2,Lian Xiang zhen 2,Huang Yu xing 2 |
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| Abstract: | 4-Methyl 5 ethoxyoxazole(Ⅰ),an important intermediate of Vitamin B 6,was synthesized through cycloaddition,hydrolysis,acidification and decarboxylation.Choosing POCl 3/Et 3N/CH 3C 6H 5/(CH 3) 2NCHO as cycloaddition and dehydration agent,when n CH 3CH(NHCOCO 2Et)CO 2Et]∶ n (POCl 3) ∶ n (Et 3N) = 1 0∶(1 0-1 2) ∶(3 5-4 2),the reaction was carried out for 8 h at 80 ℃ to give 4 methyl 5 ethoxy 2 oxazolecarboxylic acid ethyl ester(Ⅱ) in 91 7% yield.I was successfully prepared from Ⅱ in 88 2% yield through hydrolysis,acidification and decarboxylation in one pot.Analysis of the compounds was done by means of IR and 1HNMR. |
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| Keywords: | VitaminB 6 4 methyl 5 ethoxy 2 oxazolecarboxylic acid ethyl ester 4 methyl 5 ethoxyoxazole |
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