Kokristali 2,6-dihidroksibenzojske kisline z nitropiridin-N-oksidom

Franko, Patricija (author), Golobič, Amalija (mentor)

V okviru diplomskega dela smo poskusili pripraviti kokristale piridin N-oksida z benzojsko kislino, vendar sinteza ni vodila do željenih rezultatov. Poskusili smo s pripravo v več različnih topilih (etanol, diklorometan, triklorometan, tetrahidrofuran in heksan) ter z različnimi količinami reaktantov in topil. Z nadaljnjim delom pa smo uspešno pripravili kokristale 4-nitropiridin-N-oksida z 2,6-dihidrobenzojsko kislino. Rentgenska strukturna analiza na monokristalu je pokazala, da tovrstni kokristali še niso bili opisani v literaturi. Množinsko razmerje obeh izhodnih snovi je v kokristalih 1:1, pri čemer so molekule kisline preko karboksilne skupine povezane z nitrozo skupino molekul oksida z zelo močno intermolekularno vodikovo vezjo. Produkt smo karakterizirali še s pomočjo IR spektroskopije, CHN analize ter rentgenske praškovne difrakcije. Rezultati teh analiz so v skladu z rezultati strukturne analize.

• Language: Slovenian
• Keywords: Kokristali, 4-nitropiridin N-oksid, 2, 6-dihidroksibenzojska kislina, struktura
• Work type: Bachelor thesis/paper
• Typology: 2.11 - Undergraduate Thesis
• Organization: FKKT - Faculty of Chemistry and Chemical Technology
• Year: 2019
• PID: 20.500.12556/RUL-109880
• COBISS.SI-ID: 1538396355
• Publication date in RUL: 09.09.2019

Secondary language

• Language: English
• Title: Preparation and characterization of cocrystals of pyridine N-oxide and benzoic acid

Abstract

Within the diploma thesis we tried to prepare cocrystals of pyridine N-oxide with benzoic acid, but syntheses did not give desired results. We tried to prepare such cocrystals by using diffrenet solvents (ethanol, dichloromethane, trichloromethane, tetrahydrofurane and hexane) and also with different amounts of reactants and solvent. With further experimenting we were able to prepare cocrystals of 4-nitropyridine-N-oxide with 2,6-dihydrobenzoic acid. X-ray structural analysis of single-crystal of this compound showed that such cocrystals have not been known in the literature yet. Molar ratio of both starting materials withib the cocrystals is 1:1. Acid molecules are connected with oxide by very strong intermolecular hydrogen bond. Product was also characterized by IR spectroscopy, CHN analysis and X-ray powder diffraction. The results of these characterisation methods were in agreement with results of structural analysis.

• Keywords: Cocrystals, 4-nitropyridine-N-oxide, 2, 6-dihydrobenzoic acid, structure