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%
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%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2002年第4期224-226,共3页
Fine Chemicals
关键词
2-氨基-3-氰基-4-氯-5-醛基噻吩
合成
研究
染料中间体
Vilsmeier试剂
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
