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"ABSTRAKTahap awal penelitian dimulai dari pembuatan Katalis Na-ACE dari cangkang telur ayam yang diaktivasi dengan cara kalsinasi dalam suhu 950oC dan menghasilkan bubuk putih yang merupakan ACE (Activated Chicken Eggshell). ACE diimpregnasi logam Na dengan menggunakan prekursor NaOH 3% sehingga menghasilkan Na-ACE yang memiliki kebasaan lebih besar dibandingkan dengan ACE. ACE dan Na-ACE dikarakterisasi menggunakan FTIR, EDAX dan XRD serta uji kebasaan dengan metode titrasi. Na-ACE yang telah berhasil disintesis digunakan untuk sintesis chalcone yang merupakan intermediet senyawa pirazolin. Senyawa chalcone disintesis melalui mekanisme reaksi kondensasi aldol silang dengan menggunakan starting material 2-Hidroksi Asetofenon dan 2-Hidroksi Benzaldehid yang menghasilkan rendemen terbesar yaitu 84.03% pada kondisi optimum pada Suhu 60oC, selama 3 Jam dengan katalis 15%. Senyawa chalcone hasil sintesis dikarakterisasi menggunakan FTIR, UV-VIS dan LCMS. Sintesis senyawa pirazolin menggunakan senyawa chalcone hasil sintesis sebelumnya dengan hidrazin hidrat dengan perbandingan 1 : 4 yang akan menghasilkan rendemen terbesar pada kondisi optimum 4 jam reaksi, suhu 80oC dan 20% katalis dengan rendemen sebesar 62,98%. Senyawa pirazolin hasil sintesis dikarakterisasi menggunakan FTIR, UV-VIS, dan LCMS. Senyawa chalcone dan pirazolin diuji antioksidan menggunakan DPPH dan didapatkan % inhibisi chalcone sekitar 41% pada konsentrasi chalcone sebesar 1000 ppm sedangkan % inhibisi pada pirazolin sebesar 84% pada konsentrasi pirazolin sebesar 125 ppm.

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ABSTRACTThis Research was generated with the synthesis of catalyst Na-ACE from chicken egg shells, activated calcination in temperature of 950oC and will produced a white powder of ACE (Activated Chicken Eggshell). ACE was impregnated by Na metal using NaOH 3% solution as a precursor to produce Na-ACE which has a higher basicity than ACE. ACE and Na-ACE catalyst were characterized by FTIR, XRD and EDAX and for the bacisity test, titration method was used. The catalys of Na-ACE were used for synthesizing chalcone compound as intermediet material of pirazoline synthesis.Chalcone compound was synthesized through cross aldol condensation by reacting two starting materials, 2-hidroksi asetofenon, 2-hidroksi benzaldehid yield of 84,03% at the optimum condition 60oC, 3 hours and 15% catalys weight.this synthesized chalcone compound were characterized using FTIR, UV-VIS, and LCMS. The next step was synthesis pirazoline compound using chalcone and hidrazin hidrat with ratio of 1:4 and produced the greatest yield (62,98%) in the optimum conditionwhich are 4 hours reaction time, temperature of 80oC and 20% catalys weight. Pirazoline compound were characterized using FTIR, UV-VIS, and LCMS. Finally, both of chalcone and pirazoline compound were antioxidant tested using DPPH and resulted around 41% of inhibition of 1000 ppm for chalcone, and 84% inhibition of 125 ppm for pirazoline."

"Katalis basa heterogen logam natrium terimpregnasi pada kulit telur ayam teraktivasi (Na-ACE) telah berhasil disintesis dan digunakan sebagai katalis dalam reaksi kondensasi aldol. Katalis Na-ACE hasil sintesis dikarakterisasi dengan instrumen FTIR, XRD, serta uji kebasaan. Optimasi sintesis analog chalcone yaitu [1-(2-hidroksifenil)-3- (3-metoksifenil) prop-2-en-1-on] memperoleh kondisi reaksi optimum dengan 30% berat katalis, suhu reaksi 60oC, waktu reaksi 180 menit dengan pelarut etanol. Yield terbesar yang diperoleh adalah 57,22% dengan kemurnian kristal 99,85% menggunakan TLC Scanner. Chalcone hasil sintesis dikarakterisasi dengan FTIR, UV-VIS, LC-MS. Derivat Senyawa chalcone yaitu pirazolin berhasil disintesis dengan penambahan hidrazin hidrat pada kondisi refluks, suhu 70°C, reaksi selama 24 jam dan penambahan katalis Na-ACE 30%. Hasil sintesis dikarakterisasi dengan instrumen FTIR, UV-VIS, LC-MS dan H-NMR. Uji aktivitas antioksidan secara in-vitro dilakukan pada analog chalcone dan pirazolin hasil sintesis dengan metode radikal DPPH. IC50 senyawa analog chalcone sebesar 966,41 µg/ml, sedangkan IC50 senyawa pirazolin sebesar 26,84 µg/ml.

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Heterogeneous base catalyst sodium impregnated on activated chicken eggshell (Na-ACE) has been prepared and used for the aldol condensationreaction. Na-ACE was characterized by FTIR, XRD, and basicity test. The variables used for the syntheses of chalcone analogue were % catalyst mass, reaction temperature, reaction time and solvent. The highest yield (57,22% with 99,85% of purity) has been obtained under 30% catalyst mass were added, reaction temperature of 60oC, reaction time of 180 minuteswith ethanol as a solvent.

Pyrazoline as a chalcone derivative was synthesized by reacting chalcone with hydrazine hydrate and Na-ACE under reflux condition for 24 hour, reaction temperature of 70°C in ethanol. The structures and exact mass of the product were confirmed by spectral data FTIR, UV-VIS, LC-MS and H-NMR. Analogue chalcone and pyrazoline have been tested for their antioxidant activities (1,1-biphenyl-2-picrylhydrazyl free radical scavenging method). Both of the them showed activity with IC50 at 966,41 µg/ml and 26,84 µg/ml for the analogues chalcone and pyrazoline respectively."