4-氰基苯甲酸酐的合成

Synthesis of 4-cyan-o-phthalic anhydride

以偏苯三甲酸酐和氯化亚砜为原料 ,其摩尔比为 1:1 2 ,在回流状态下首先合成中间体 4 -氯甲酰基苯甲酸酐Ⅱ ,产率可达 98%。Ⅱ经过胺化、减压脱水制得 4 -氰基苯甲酸酐 ,其沸点为 175～ 180 C/ 0 2 6KPa ,各反应物摩尔比为n (Ⅱ ) :n (NH3 ) :n (P2 O5) =1 0 :4 7:2 1。通过红外分析、1H -NMR分析及元素分析证明 ,所得到的化合物即为目标物。

Chloroformylphthalic anhydride(Ⅱ) is synthesized from trimellitic anhydride and thionyl chloride with refluxing,and mole ratio of trimellitic anhydride/thionyl chloride is 1:1.2,the yield is 98%.4-cyan-o-phthalic anhydride is synthesized from 4-chloroformylphthalic anhydride by aminating then dehydration with decompressing,its boiling point is 175～180°C/0.26kPa,the total yield is 70%,the mole ratio of reactant is n (Ⅱ):n(NH 3):n(P 2O 5)=1.0:4.7:2.1.It is characterized by IR? 1H-NMR and element analysis.