Satria Rizky Azhar, - and Asep Kadarohman, - and Ratnaningsih Eko Sardjono, - (2025) OPTIMASI EPOKSIDASI β-KARIOFILEN DENGAN HIDROGEN PEROKSIDA DALAM ETANOL. S1 thesis, Universitas Pendidikan Indonesia.
Abstract
Kariofilen oksida dapat disintesis dari β-kariofilen tanpa katalis menggunakan oksidator hidrogen peroksida (H2O2) dalam pelarut etanol. Penelitian ini bertujuan mengoptimasi, memahami mekanisme reaksi, mengetahui metode pemisahan dan pemurnian, menentukan rendemen dan kemurnian, serta karakterisasi. Optimasi dilakukan dengan memvariasikan suhu, jumlah mol ekuivalen H2O2 dan waktu reaksi. Sintesis dilakukan dengan pelarutan β-kariofilen ke dalam etanol, pemanasan, penambahan H2O2 50% dan perlakuan refluks. Campuran reaksi diekstraksi dengan n-heksana dua kali dan diuapkan dengan destilasi atau didiamkan pada suhu ruang, kemudian dianalisis komponennya menggunakan GC-FID. Proses pemisahan dilakukan dengan antisolvent precipitation, diperoleh padatan putih tak berwarna. Pemurnian dilakukan dengan rekristalisasi sebanyak 1–2 kali menggunakan etanol. Karakterisasi dilakukan dengan analisis GC-MS, FTIR, NMR, uji titik leleh dan morfologi kristal. Kondisi optimum diperoleh pada suhu 70 °C, 8 mol ekuivalen H2O2, dan waktu 8 jam dengan persentase hasil konversi, produk utama, dan selektivitas berturut-turut sebesar 99,888%, 99,389%, dan 99,500%. Rendemen diperoleh 60,103% dengan kemurnian tertinggi 99,073%. Hasil karakterisasi GC-MS menunjukkan produk utama cocok sebagai (-)-caryophyllene oxide dengan Similarity Index (SI) tertinggi mencapai 95% dan m/z 220. Hasil spektrum FTIR oleh adanya regangan C–O dan C–O–C pada bilangan gelombang berturut-turut 1234,48–1064,74 cm⁻¹ dan 887,28 cm⁻¹ yang mengindikasikan keberadaan gugus fungsi epoksida. Hasil NMR baik spektrum 13C maupun 1H menunjukkan senyawa sebagai β-kariofilen oksida. Hasil uji titik leleh diperoleh sebesar 56°C dan morfologi kristal berbentuk ortorombik. Caryophyllene oxide can be synthesized from β-caryophyllene without a catalyst using hydrogen peroxide (H2O2) as an oxidant in ethanol solvent. This study aims to optimize, understand the reaction mechanism, determine separation and purification methods, determine yield and purity, and characterization. Optimization was carried out by varying the temperature, the molar equivalents of H2O2, and the reaction time. The synthesis was conducted by dissolving β-caryophyllene in ethanol, heating, adding 50% H2O2, and applying reflux treatment. The reaction mixture was extracted twice with n-hexane and evaporated by distillation or left at room temperature, then analyzed for its components using GC-FID. The separation process was performed by antisolvent precipitation, yielding a white, colorless solid. Purification was carried out by recrystallization 1–2 times using ethanol. Characterization was performed using GC-MS, FTIR, NMR, melting point determination, and crystal morphology analysis. The optimum conditions were obtained at 70 °C, 8 molar equivalents of H₂O₂, and 8 hours of reaction time, with conversion percentage, main product, and selectivity of 99.888%, 99.389%, and 99.500%, respectively. The yield obtained was 60.103% with the highest purity of 99.073%. GC-MS characterization indicated that the main product matches (-)-caryophyllene oxide, with a highest Similarity Index (SI) of 95% and m/z 220. FTIR spectra showed C–O and C–O–C stretching at 1234.48–1064.74 cm⁻¹ and 887.28 cm⁻¹, indicating the presence of epoxide functional groups. Both 13C and 1H NMR spectra confirmed the compound as β-caryophyllene oxide. The melting point was determined to be 56 °C, and the crystal morphology was orthorhombic.
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| Item Type: | Thesis (S1) |
|---|---|
| Additional Information: | https://scholar.google.com/citations?view_op=new_profile&hl=en ID SINTA Dosen Pembimbing: Asep Kadarohman: 5984423 Ratnaningsih Eko Sardjono: 5979503 |
| Uncontrolled Keywords: | β-Kariofilen, Kariofilen oksida, Epoksidasi, Hidrogen peroksida, Reaksi tanpa katalis β-Caryophyllene, Caryophyllene oxide, Epoxidation, Hydrogen peroxide, Catalyst-free reaction |
| Subjects: | Q Science > Q Science (General) Q Science > QD Chemistry |
| Divisions: | Fakultas Pendidikan Matematika dan Ilmu Pengetahuan Alam > Program Studi Kimia - S1 > Program Studi Kimia (non kependidikan) |
| Depositing User: | Satria Rizky Azhar |
| Date Deposited: | 11 Sep 2025 03:24 |
| Last Modified: | 11 Sep 2025 03:24 |
| URI: | http://repository.upi.edu/id/eprint/138484 |
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