Susy Yunita Prabawati
Program Studi Kimia, Fakultas Sains dan Teknologi, UIN Sunan Kalijaga Yogyakarta Jl. Laksda Adisucipto, Yogyakarta

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Grinding Technique on Synthesis of Calixarene and Its Derivatives Prabawati, Susy Yunita; Mufidati, Afifah; Ratna Djuwita, Titis; Ratna Djuwita, Titis; Nur Ngaini, Siti
EKSAKTA: Journal of Sciences and Data Analysis VOLUME 1, ISSUE 2, August 2020
Publisher : Fakultas Matematika dan Ilmu Pengetahuan Alam

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.20885/EKSAKTA.vol1.iss2.art4

Abstract

The synthesis of p-t-butylcalix[6]arene (PK[6]A) and calixresorcinarene derivative compounds, namely C-para-dimethylamino-phenylcalix[4]resorcinarene (CPDAK[4]R) and C-4-hydroxy-phenylcalix[4]-resorcinarene (CHK[4]R), had been carried out by grinding technique. The grinding technique was done with the absence of solvents so that it minimized the waste. Synthesis occurred through electrophilic substitution reactions with KOH as an alkaline catalyst and p-toluene sulfonic acid as an acid catalyst. The three calixarene products were in the form of crystalline solids with a melting point of more than 300°C, insoluble in water with yields of 62.58; 61.94 and 97.49%, respectively. Product characterization using FTIR analysis showed the vibration of the methylene bridge (-CH2-) at a wavenumber of 1473.62 cm-1 and LC-MS analysis for (PK[6]R) showed that the molecular weight was 974.77 g/mole. While the analysis of (CPDAK[4]R) and (CHK[4]R) with 1H NMR showed the presence of protons from the methine bridge (-CH-) that appear at the chemical shift of  4.950 and 3.078 ppm.
Sintesis Senyawa Mentil Vanilat dari Vanilin dan Aplikasinya sebagai Parfum Risnandar, Ade Irfan; Prabawati, Susy Yunita
ALKIMIA Vol 3 No 2 (2019): ALKIMIA
Publisher : SCIENCE AND TECHNOLOGY FACULTY OF UNIVERSITAS ISLAM NEGERI RADEN FATAH PALEMBANG

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (272.504 KB) | DOI: 10.19109/alkimia.v3i2.3805

Abstract

Synthesis of menthyl vanilate compound has been carried out and its application asperfume. The synthesis was carried out through oxidation of vanillin using Tollens reagentfollowed by esterification of vanillic acid with menthol. The result of oxidation process wereanalyzed for melting point and characterized using FTIR. Esterification of vanillic acid usingmenthol was carried out by addition of SOCL2 reagent. The synthesized compound wascharacterized using FTIR and Proton Nuclear Magnetic Resonance (1H-NMR) and followedby organoleptic test. Melting point of vanillic acid is 212oC. Identification of vanillic acidwith FTIR is shown that the absorption of C-H aldehyde at wave numbers 2850 and 2750 cm -1 is absence indicating that the aldehyde group of vanillin has been oxidized completely.Esterification of Vanillic acid using menthol with the addition of SOCl2 produces anirreversible reaction and obtained a brown liquid which is mentil vanilat ester compound.Synthesis of menthyl vanilate compound was obtained with yield 48.05%. Identification ofmenthyl vanillate with FTIR showed the absorption of C-O (from Ester) at wave numbers1219 and 1180 cm-1. Identification with 1H NMR showed the peak at chemical shift 0.74-2.16 ppm which is absorption of proton from the substituted menthyl group. Based on theresult of identification using FTIR and 1H NMR spectrophotometers can be concluded thatmenthyl vanillate compound has been successfully synthesized. The result of organoleptic testshowed that 95% of respondents agree that the compound is fragrant, 100% respondents agreethat the the aroma of compound is sharp, and 75% of respondents like the product of thesynthesized compound to be perfume.