CAJ | 학술논문

以α-甲基苯乙烯（α-MS）为原料,分别高选择性地合成了-MS线性二聚体（Ⅰ）和α-MS环状二聚体（Ⅱ）,并再以Ⅱ为原料,两步法合成了光引发剂KIP150（Ⅲ）。研究结果表明,以对甲苯磺酸为催化剂,在30℃下反应24h,产物Ⅰ收率88.0%,纯度大于99.8%;同样以对甲苯磺酸为催化剂,在100℃下反应7 h,产物Ⅱ收率98.0%,纯度大于99.8%;化合物Ⅱ经酰基化反应和羟基化反应即可得产物Ⅲ,总收率高于70.0%,纯度可达95.0%以上。实验中采用LC-MS、1H NMR、GC、HPLC等分析方法对各反应产物进行结构确定和纯度测定。
이α-갑기분을희（α-MS）위원료,분별고선택성지합성료-MS선성이취체（Ⅰ）화α-MS배상이취체（Ⅱ）,병재이Ⅱ위원료,량보법합성료광인발제KIP150（Ⅲ）。연구결과표명,이대갑분광산위최화제,재30℃하반응24h,산물Ⅰ수솔88.0%,순도대우99.8%;동양이대갑분광산위최화제,재100℃하반응7 h,산물Ⅱ수솔98.0%,순도대우99.8%;화합물Ⅱ경선기화반응화간기화반응즉가득산물Ⅲ,총수솔고우70.0%,순도가체95.0%이상。실험중채용LC-MS、1H NMR、GC、HPLC등분석방법대각반응산물진행결구학정화순도측정。
Linear dimer,product（Ⅰ） and cyclic dimer,product（Ⅱ） of α-methyl styrene（α-MS） were synthesized with high selectivity from α-MS,and macromolecular photoinitiator KIP150,product（Ⅲ） was prepared from α-MS cyclic dimer in two steps.The results indicated that in the presence of p-toluenesulfonic acid,the yield of product（Ⅰ） was more than 88.0% and the purity was up to 99.8% at reaction temperature 30 ℃ for 24h.Moreover,in the presence of p-toluenesulfonic acid and at reaction temperature 100 ℃ for 7h,the yield of product（Ⅱ） was up to 98.0% and the purity was more than 99.8%.The yield of product（Ⅲ） was more than 70.0% when synthesized via Friedel-Crafts acylation and hydroxylation reaction with α-MS cyclic dimer,and the purity was up to 95.0%.The products and intermediates were characterized by LC-MS,1H NMR,GC and HPLC.