6-氨基-1,2-苯并吡喃酮的制备及表征

PREPARATION AND CHARACTERIZATION OF 6-AMINO-1,2-BENZOPYRONE

以80%水合肼为还原剂、FeCl_3/C为催化剂,还原6-硝基-1,2-苯并吡喃酮制备6-氨基-1,2-苯并吡喃酮,并通过~1 H NMR、IR、^(13)C NMR和LC-MS表征了目标产物的结构,HPLC分析纯度达99%以上。同时探究了水合肼用量、反应温度、反应时间以及催化剂用量对反应的影响。较佳的合成工艺条件为:n(80%水合肼)∶n(6-硝基-1,2-苯并吡喃酮)=2.5,FeCl_3用量为0.8g,活性炭用量为0.2g,反应温度为78℃,反应时间3.5h,收率可达85.0%。

6-Amino-1,2-benzopyrone was prepared using 80% hydrazine hydrate as reducing agent and FeCl3/C as catalyst,and the structure was confirmed by ～1 H NMR,IR,^13C NMR and LC-MS,the purity of the product was over 99%.Also the effects of hydrazine hydrate dosage,reaction temperature,reaction time and catalyst dosage were discussed.The results showed that the optimal conditions were：n（80% hydrazine hydrate）∶n（6-nirio-1,2-benzopyrone）=2.5,FeCl3 0.8 g,activated carbon 0.2 g,reaction temperature 78 ℃,reaction time 3.5 h,and the yield of the product was 85.0%.