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Gxxxxx Experimental Chemicals. Phthalic anhydride, β-alanine, glacial acetic acid, ether, Chloroform, were obtained from merck Chemical Co. The infrared.

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Presentation on theme: "Gxxxxx Experimental Chemicals. Phthalic anhydride, β-alanine, glacial acetic acid, ether, Chloroform, were obtained from merck Chemical Co. The infrared."— Presentation transcript:

1 gxxxxx Experimental Chemicals. Phthalic anhydride, β-alanine, glacial acetic acid, ether, Chloroform, were obtained from merck Chemical Co. The infrared spectra in the range 400–4000 cm −1 were recorded on a Shimadzu FTIR-8400S spectrophotometer. UV spectrophotometer (ShimadzuUV-1700) was used. 1 H NMR spectra were recorded in CDCl3 with (300 MHz) Spectrometer using of TMS as an internal reference. A MW oven by setting the power range to medium high(70% of total power). scanning electron microscopy(SEM). Synthesis of N-Phthaloyl-(β)-alanine with normal reflux conditions: (β)-Alanine (1) (3.238 gr) and phthalic anhydride (2) (5.385 g) were heated under reflux in glacial acetic acid (32.5 mL) for 3 h (bath temperature =118 °C). The acetic acid was evaporated under vacuum. Water (7 mL) was added to the residue and the mixture was refluxed for 1 hour. After cooling, the resulting mixture was extracted with ether-water (1 : 4). The precipitated solid was filtered and dried under vacuum to give white crystals of the title compound (3) (7.32 g). Yield = 89.6 %. M. p =150°C. Synthesis of N-Phthaloyl-(β)-alanine with Microwave: Mixture of phthalic anhydride (1.481gr) and (β)-Alanine (0.8909 gr) was placed in a Erlenmeyer flask with a loose top cap and heated in microwave by setting the power range in medium high (70% of total power) after 10 minutes reaction mixture tested with TLC method and again put the flask in microwave and heated for 5 minutes and tested with TLC. After cooling, the reaction mixture was extracted with water-chloroform (1-3), dried (Na 2 SO 4 ), filtered and the solvent removed. Yield = 93.6 %. M. p =146. Results References [1] Helen J. Kitchen et al, Chem.Rev,114(2014)1170. [2] Osman et al, Chemistry Central Journal ( 2012) 2. [2]Mostafa Baghbanzadeh, et al, Angew. Chem. Int. Ed, 50( 2011) 1312. [3] Bhupinder Singh Sekhon, International Journal of PharmTech Research, 2(2010) 827. [4] C. Oliver Kappe, Angew. Chem. Int. Ed, 43(2004) 6250. [5] Adamo Fini, Alberto Breccia, Pure Appl. Chem., 71(1999) 573. [6] Radia Mahboub, Int. J. Chem. Sci.,7( 2009) 28. Fig.1. UV-Vis absorption spectrum Fig.2. FT-IR Spectrum Table1. Proton NMR Spectrum Fig.3. SEM images of N-Phthaloyl-(β)-alanine(a-c) sample.A prepared by CCM (d-f) sample B prepared by MCM a b c d e f Conclusion In the present work, N-Phthaloyl-(β)-alanine was prepared by CCM and MCM. The formation of N-Phthaloyl-(β)-alanine was confirmed by using UV-Vis, FT-IR, and 1 H NMR spectroscopy. In CCM, the reaction was completed only after 3 h, where as in MCM, the reaction was completed within few minutes.Within the limited time, nucleation and growth had to be finished. Hence, the particles with smaller and narrow distribution were obtained by MCM. However, in CCM, the time might be sufficient to form the separate phases, which has led to the bigger particle size. Relative to conventional methods, the microwave approach significantly reduced synthesis time and amounts of reagents and It is a clean, cheap method. Moreover, it is environment-friendly, simple to operate, and energy efficient over the conventional combustion methods The formation of N-Phthaloyl-(β)-alanine was confirmed by SEM.


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