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α-甲基苯乙烯二聚体的合成及应用

宋国强1,金晓蓓1,胡春青2,陈 昕1   

  1. 1常州大学制药与生命科学学院,江苏 常州 213164;2常州强力电子新材料股份有限公司,江苏 常州 213011
  • 出版日期:2012-09-05 发布日期:2012-09-05

Synthesis and application of α-methyl styrene dimer

SONG Guoqiang1,JIN Xiaobei1,HU Chunqing2, CHEN Xin1   

  1. 1School of Pharmacy & Life Science,Changzhou University,Changzhou 213164,Jiangsu,China; 2Changzhou Tronly New Electronic Materials Co.,Ltd.,Changzhou 213011,Jiangsu,China
  • Online:2012-09-05 Published:2012-09-05

摘要: 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。

关键词: 关键词:α-甲基苯乙烯(α-MS), α-MS线性二聚体, α-MS环状二聚体, 大分子光引发剂, KIP150, α-甲基苯乙烯, α-MS线性二聚体, α-MS环状二聚体, 大分子光引发剂, KIP150

Abstract: 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.

Key words: Key words: α-methyl styrene(α-MS), α-MS linear Dimer, α-MS cyclic Dimer, Macromolecular photoinitiator, KIP150, α-methyl styrene(α-MS), α-MS linear dimer, α-MS cyclic dimer, macromolecular photoinitiator, KIP150

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