scholarly journals SYNTHESIS OF SAFRYL KETONE FROM SAFROLE

2010 ◽  
Vol 4 (1) ◽  
pp. 58-61
Author(s):  
Hanoch J Sohilait ◽  
Hardjono Sastrohamidjojo ◽  
Sabirin Matsjeh ◽  
J Stuart Grossert
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
1H Nmr ◽  
Mass Spectroscopy ◽  
Structure Elucidation ◽  
Secondary Alcohol ◽  
Proton Nuclear Magnetic Resonance ◽  
Infra Red ◽  
Nuclear Magnetic

Synthesis of safryl ketone from safrole has been achieved through conversion of allyl group to secondary alcohol, followed by oxidation with PCC-Al2O3. The oxymecuration-demercuration reaction of safrole with HgSO4-NaBH4 yields safryl alcohol (66.38%) and the oxidation of safryl alcohol with PCC-Al2O3 yields safryl ketone (62.92%). The structure elucidation of these products was conducted using Fourier Transformed Infra Red Spectroscopy (FTIR), Proton-Nuclear Magnetic Resonance (1H-NMR) and Mass Spectroscopy (MS).   Keywords: safryl ketone, safrole

Immunosuppressive activity of cyclosporine metabolites compared and characterized by mass spectroscopy and nuclear magnetic resonance

1990 ◽  
Vol 36 (2) ◽  
pp. 225-229 ◽  
Author(s):  
K R Copeland ◽  
R W Yatscoff ◽  
R M McKenna
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Mass Spectroscopy ◽  
Proton Nuclear Magnetic Resonance ◽  
Therapeutic Monitoring ◽  
Potency Ratio ◽  
Transplant Patients ◽  
In Vitro Systems ◽  
Nuclear Magnetic

Abstract Eight cyclosporine (CsA) metabolites were isolated from the urine of renal-transplant patients by high-pressure liquid chromatography. Structure and purity of the metabolites were assessed by fast atomic bombardment/mass spectroscopy, by proton nuclear magnetic resonance (NMR), and, when the quantity of metabolites permitted, by 13C-NMR. The immunosuppressive activities (I) of the metabolites were tested in three separate in vitro systems: primary and secondary mixed lymphocyte reactions as well as by a mitogen-stimulated system. The I, as measured by comparing the concentration of each metabolite required for 50% inhibition of incorporation of [3H] thymidine, varied among the assay systems, as did the ranking of I among the test systems. In general, the I of most metabolites in all assay systems were less than 10% of that for CsA. Metabolites with single modifications exhibited the greatest I; e.g., that of M-17 was congruent to 16% of that of CsA (potency ratio 0.16) in a secondary mixed lymphocyte reaction. The significance of these findings in relation to therapeutic monitoring of CsA is discussed.

Thermal-oxidation study of biodiesel by proton nuclear magnetic Resonance (1H NMR)

Fuel ◽  
2020 ◽  
Vol 274 ◽  
pp. 117833
Author(s):  
Ana Carolina Gomes Mantovani ◽  
Letícia Thaís Chendynski ◽  
Diego Galvan ◽  
Fernando César de Macedo Júnior ◽  
Dionísio Borsato ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Thermal Oxidation ◽  
1H Nmr ◽  
Proton Nuclear Magnetic Resonance ◽  
Oxidation Study ◽  
Nuclear Magnetic

Use of high-resolution proton nuclear magnetic resonance spectroscopy for rapid multi-component analysis of urine.

1984 ◽  
Vol 30 (3) ◽  
pp. 426-432 ◽  
Author(s):  
J R Bales ◽  
D P Higham ◽  
I Howe ◽  
J K Nicholson ◽  
P J Sadler
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Magnetic Resonance ◽  
High Resolution ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Proton Nuclear Magnetic Resonance ◽  
Resonance Spectroscopy ◽  
Simple Method ◽  
Nuclear Magnetic

Abstract Numerous low-Mr metabolites--including creatinine, citrate, hippurate, glucose, ketone bodies, and various amino acids--have been identified in 400- and 500-MHz proton nuclear magnetic resonance (1H NMR) spectra of intact human urine. The presence of many of these was related to the specific condition of the donors: humans in different physiological states (resting, fasting, or post-exercise) and pathological conditions (e.g., diabetes mellitus, cadmium-induced renal dysfunction). We have also monitored the metabolism of simple nonendogenous compounds (methanol and ethanol) and of acetaminophen. The pH-dependencies of the NMR chemical shifts of some urine components are reported. Our studies show that high-resolution 1H NMR spectroscopy provides a fast, simple method for "fingerprint" identification of urinary compounds. In some cases, analytes can be quantified by standard additions or by comparing integrated peak areas for the metabolites with those for creatinine. Determinations of creatinine by 1H NMR spectroscopy compared well with those by an independent chemical assay based on the Jaffé reaction.

Structural Study of Nicotine Salts

1983 ◽  
Vol 12 (2) ◽  
Author(s):  
T.A. Perfetti
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Ultra Violet ◽  
Dicarboxylic Acids ◽  
Acid Group ◽  
Proton Nuclear Magnetic Resonance ◽  
Monocarboxylic Acids ◽  
Pyridine Group ◽  
Infra Red ◽  
Nuclear Magnetic

AbstractThe structures of three types of nicotine salts have been determined. These salts have acid to base ratios of either 1 : 1, 2 : 1, or 3 : 1. Salt formation between organic acids and nicotine is dependent upon the structure of the acids (aliphatic or aromatic) and their functionality. The 1 : 1 salts of nicotine have amino acids or benzoic-type acids bound to the N-methylpyrrolidine nitrogen of nicotine. The 2 : 1 salts are found to bind to one acid group as in the 1 : 1 salts and a second to the nitrogen of the pyridine ring. The 2 : 1 salts of nicotine are formed with formic acid, aliphatic dicarboxylic acids, and/or nitroaromatic acids. Nicotine forms 3 : 1 salts with aliphatic monocarboxylic acids starting with acetic acid. Here one acid is bound as in the 1 : 1 salts while the other two acids dimerize and bind to the nitrogen of the pyridine group. Infra-red (IR), ultra-violet (UV), proton nuclear magnetic resonance (PMR), and carbon nuclear magnetic resonance (CMR) spectroscopy as well as field desorption - mass spectroscopy (FD-MS) were used in this investigation of the structure of nicotine salts.

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