| 2-氨基-3-氰基-4-氯-5-醛基噻吩的合成研究 |
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| 引用本文： | 简卫,程侣柏.2-氨基-3-氰基-4-氯-5-醛基噻吩的合成研究[J].精细化工,2002,19(4):224-226. |
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| 作者姓名： | 简卫 程侣柏 |
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| 作者单位： | 大连理工大学精细化工国家重点实验室,辽宁,大连,116012 |
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| 摘 要： | 以 2 氨基 3 氰基 4 ,5 二氢噻吩 4 酮 (ACDHTO)与Vilsmeier试剂反应得到 2 (N ,N 二甲基甲脒基 ) 3 氰基 4 氯 5 醛基噻吩 ,然后在酸性条件下水解得到 2 氨基 3 氰基 4 氯 5 醛基噻吩。确定了 2 (N ,N 二甲基甲脒基 ) 3 氰基 4 氯 5 醛基噻吩的反应条件为 :n(POCl3 )∶n(ACDHTO)=3 0∶1 0 ,ACDHTO的质量 (g)与DMF的体积 (mL)之比为 1 0∶5 7,在 70～ 75℃下反应 6h ,收率达到 95 2 % ,质量分数为 97 9% ,两步总收率为 89 3%
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| 关 键 词： | 2氨基3氰基4 5二氢噻吩4酮 2(N N二甲基甲脒基)3氰基4氯5醛基噻吩 2氨基3氰基4氯5醛基噻吩 Vilsmeier试剂 |
| 文章编号： | 1003-5214(2002)04-0224-03 |
Synthesis of 2-Amino-3-cyano-4-chloro-5-formylthiophene |
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| Abstract: | Amino 3 cyano 4 chloro 5 formylthiophene was synthesized through a two step process. 2 Amino 3 cyano 4,5 dihydrothiophen 4 one(ACDHTO) reacted with Vilsmeier reagent to give 2 ( N,N dimethylformamidino) 3 cyano 4 chloro 5 formylthiophene, which was then hydrolysed to provide the product. The optimum reaction conditions of the first step were detemined. With n (POCl 3)∶ n (ACDHTO)=3 0∶1 0 and weight(g) of ACDHTO:volume(mL) of DMF=1 0∶5 7,the reaction was carried out at 70-75 ℃ for 6 h to give 2 ( N,N dimethylformamidino) 3 cyano 4 chloro 5 formylthiophene in 95 2% yeild and of 97 9% purity.Total yield of two steps was 89 3%. |
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| Keywords: | amino 3 cyano 4 chloro 5 formylthiophene 2 amino 3 cyano 4 5 dihydrothiophen 4 one 2 ( N N dimethylformamidino) 3 cyano 4 chloro 5 formylthiophene Vilsmeier reagent |
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