论文部分内容阅读
以咔唑为起始原料,通过N-烷基化、酰化、羟胺化、酯化反应,合成了咔唑肟酯类光引发剂OXE-2,并用1HNMR、MS、HPLC对各步反应产物进行了表征。考察了影响各步反应收率的主要因素和纯化方法,最终反应总收率为45.0%。经重结晶,可使最终产物相对质量分数达99.2%。用“一锅煮”法完成了不对称酰化反应,简单、可靠,最终可使不对称酰化产物收率和相对质量分数分别达到71.8%和97.8%,较佳反应投料比是:n(N-乙基咔唑)∶n(AlCl3)∶n(邻甲基苯甲酰氯)∶n〔AlCl3(二次投料)〕∶n(乙酰氯)=1∶1.1∶1.06∶1.1∶1.29。
The carbazole oxime ester photoinitiator OXE-2 was synthesized by N-alkylation, acylation, hydroxylamine and esterification using carbazole as starting material. The reaction products of each step Characterized. The main factors affecting the yield of each reaction step and the purification method were investigated. The final reaction yield was 45.0%. After recrystallization, the final product relative mass fraction of 99.2%. The asymmetric acylation reaction was completed by the “one-pot” method, which was simple and reliable. The yield and the relative mass fraction of the asymmetric acylation products reached 71.8% and 97.8% respectively. The best reaction feed ratio was n (AlCl3): n (o-methylbenzoyl chloride): n [AlCl3 (secondary charge)]: n (acetyl chloride) = 1: 1.1: 1.06: 1.1: 1.29.