Improved Synthesis of the Isobutyrylbenzene of the Key Intermediate of Photoinitiator D-1173
College of Chemical and Biological Engineering, Zhejiang University, Zhejiang Provincial Key Laboratory of Advanced Chemical Engineering Manufacture Technology, Hangzhou 310027, China
Abstract: 2-hydroxy isobutyrylbenzene (D-1173) is a typical free radical photoinitiator widely used in UV curing systems. Isobutyrylbenzene is the key intermediate in the synthesis of D-1173. An improved synthesis process for isobutyrylbenzene was studied via Grignard reaction with benzonitrile and 2-chloropropane as starting material. The optimized process conditions were as follows: synthesis of isopropyl magnesium chloride: molar ratio of 2-chloropropane to magnesium 1.0:1.1, tetrahydrofuran as solvent, 40 ℃ for 2 h, iodine as initiator; synthesis of isobutyrylbenzene: molar ratio of benzonitrile to isopropyl magnesium chloride 1.0:1.1, 0 ℃ for 2 h, The amount of cuprous bromide added as a catalyst was 1% (molar fraction, based on benzonitrile). Compared with Friedel-Crafts acylation process, this process avoids the use of aluminium chloride, which is more environmental-friendly and has good industrial application value.
XU Ze,FEIDAWASI Adili,CHEN Xinzhi et al. Improved Synthesis of the Isobutyrylbenzene of the Key Intermediate of Photoinitiator D-1173[J]. 化学反应工程与工艺, 2019, 35(3): 227-233.