AlCl_3催化下合成1,2-蒽乙二酮

Synthesis of 1,2-aceanthrylenedione catalyzed by AlCl_3

研究了以高活性Lewis酸无水三氯化铝(AlCl3)为催化剂,蒽和草酰氯为反应物合成1,2-蒽乙二酮的酰基化反应。用GC考察了不同反应条件对1,2-蒽乙二酮产率的影响,当蒽为1 mmol,草酰氯为2 mmol,AlCl3为4 mmol,溶剂为CS2(15mL),反应温度为30℃,反应时间5 h的条件下,1,2-蒽乙二酮的产率最高,为83.8%。通过萃取、重结晶等方法得到了1,2-蒽乙二酮纯品,用熔点测定、GC/MS、FT-IR和1HNMR等分析测试手段鉴定了其结构。

1,2-Aceanthrylenedione was synthesized through the acylation reaction of anthracene and oxalyl chloride catalyzed by anhydrous AlCl3. The effect of various reaction conditions on the yield of 1,2-aceanthrylenedione was studied by C,C analysis.The results showed that the optimum synthesis conditions of the acylation reaction in the presence of CS2（15 mL） as the solvent of the reaction were as follows ：4 mmol of anhydrous AlCl3, a molar ratio of 1 ： 2 between oxalyl chloride and anthracene, a reaction time of 5 h and a： reaction temperature of 30 ℃. Under these conditions, the yield of 1,2-aeeanthrylenedione was 83.8 % . Pure 1,2- aeeanthrylenedione was prepared through extraction and reerystallization of raw compound and the structure of 1,2-aeeanthrylenedione was identified by melting point measurement, GC/MS, FTIR and 1^HNMR analyses.