Chemical Properties
Density 1.183 g/cm3, melting point 88-90°C (lit.), boiling point 405℃ at 760 mmH, flash point 155.8℃, refractive index .544, vapor pressure 2.75E-07 mmHg at 25℃.
Synthesis
The general procedure for the synthesis of photoinitiator 2959 from the compound (CAS:159119-01-4) was as follows: a 25 mL Schlenk reaction tube was taken and N-bromosuccinimide (NBS) 18 mg (0.1 mmol) was added sequentially as catalyst, 4'-(2-hydroxyethoxy)-2-methylpropiophenone 105 mg (0.5 mmol), and dimethyl sulfoxide (DMSO) 1 mL as oxidizing reagent and solvent. ), and dimethyl sulfoxide (DMSO) 1 mL as oxidizer, carbonylation reagent and solvent. The reaction mixture was stirred at 100 °C for 24 hours. Upon completion of the reaction, 15 mL of ethyl acetate and 3 mL of brine were added to the reaction mixture for extraction, which was then extracted three times with ethyl acetate. All organic phases were combined and purified by column chromatographic separation to give a final purity of 103 mg of 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone in 92% yield.
References
[1] Organic Letters, 2015, vol. 17, # 4, p. 876 - 879
[2] Patent: CN104710256, 2017, B. Location in patent: Paragraph 0174-0177
[3] Angewandte Chemie - International Edition, 2014, vol. 53, # 2, p. 548 - 552
[4] Angew. Chem., 2014, vol. 53, # 2, p. 558 - 562,5
[5] Patent: CN107739303, 2018, A. Location in patent: Paragraph 0017