Synthesis of Ortho Phthaloyl Chloride Using Triphosgene by Response Surface Methodology

Abstract:

A simple approach for the synthesis of Ortho Phthaloyl Chloride(OPC) was studied .Response surface methodology (RSM) was used to optimize the synthesis conditions of OPC. A 4-factor central composite design (CCD) was used for experimental design and analysis to obtain the optimal processing parameters, such as amount of triphosgene(BTC), amount of catalyst, reaction temperature and time. The 3-D response surface and the contour plots derived from the mathematical models were applied to determine the optimal conditions. The optimum reaction conditions were as follows: amount of BTC 62 g, amount of cat. 3.3 g, reaction temperature 75°C, reaction time 5 h. Under these conditions, The yield of OPC was 96.61%. Comparison of predicted and experimental values revealed good correspondence, implying that empirical model could be used to adequately describe the relationship between the factors and response in OPC synthesis process.

• Periodical: Advanced Materials Research (Volumes 634-638)
• Pages: 3026-3032
• DOI: https://doi.org/10.4028/www.scientific.net/AMR.634-638.3026
• Online since: January 2013
• Authors: Xuan Tang, Xi Tao Cheng, Feng Lin Huang
• Keywords: Ortho Phthaloyl Chloride, Response Surface Methodology (RSM), Synthesis, Triphosgene

References

[1] L.P. Kyrides. Phthalyl Chloride, J. Am. Chem. Soc. 1 206-208, (1937).

[2] Qiu Wei-Jun. The Synthesis of Phthalyl Chloride, Ningbo Chemical Indistry. 1 35, (1997).

[3] Shieh CJ, Akoh CC, Koehler PE. Four-factor response surface optimization of the enzymatic modification of triolein to structured lipids, J Am Oil Chem Soc. 72 6-10, (1995).

DOI: 10.1007/bf02635645

[4] Soo EL, Salleh AB, Basri M, Rahman RNZA, Kamaruddin K. Response surface methodological study on lipase-catalyzed synthesis of amino acid surfactants, Process Biochem 39 1511–1518, (2004).

DOI: 10.1016/s0032-9592(03)00279-6

[5] Xiuqing Kang. Study on the Synthesis of Imidacloprid's Intermediate 2-Chlorl-5-Methyl-Pyridne, Scientific Dissertation of Beijing University of Chemical Technology(2004).

[6] Chunlin Ye, Chengjun Jiang. Optimization of extraction process of crude polysaccharides from Plantago asiatica L by response surface methodology, Carbohydrate Polyers. 84 495-502, (2011).

DOI: 10.1016/j.carbpol.2010.12.014

[7] Adinarayana, K., Ellaiah, P. Response surface optimization of the critical medium components for the production of alkaline protease by a newly isolated Bacillus sp, Journal of Pharmacy and Pharmaceutical Sciences. 3 272-278, (2002).

[8] Wu, D., Zhou, J., Li, Y. Effect of the sulfidation process on the mechanical properties ofaCoMoP/Al2O3 hydrotreating catalyst, Chemical Engineering Science. 2 198-206, (2009).

DOI: 10.1016/j.ces.2008.10.014

[9] Juan Mao, Shi Yn Lee , Sung Wook Won, Yeoung-Sang Yun. Surface modified bacterial biosorbent with poly(allylamine hydrochloride): Development using response surface methodology and use for recovery of hexachloroplatinate(IV) from aqueous solution, Water research. 44 5919-5928, (2010).

DOI: 10.1016/j.watres.2010.07.034