BazTech - Yadda

1

Derywatyzacja w chromatografii gazowej. Przegląd metod i reagentów

Haliński Łukasz

Laboratorium - Przegląd Ogólnopolski

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2020

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nr 3

14--21

PL

Synteza pochodnych (derywatyzacja) to kluczowy etap wielu metod analitycznych wykorzystujących chromatografię gazową. Pozwala na zwiększenie lotności oraz stabilności termicznej analitów, a także ułatwia identyfikację substancji. W artykule przedstawione są najważniejsze metody syntezy pochodnych oraz przegląd powszechnie stosowanych reagentów. Wskazane są także możliwe drogi rozwoju analityki w tym obszarze.

EN

Derivatization is a key stage of many analytical procedures that utilize gas chromatography as an analytical technique. lt enables increasing the volatility and thermal stability of analytes, and sometimes facilitates their identification. The most important methods of derivatization and widely used reagents are described in this short review. Perspectives of the further progress in this field are also briefly discussed.

2

Acylation of aromatic compounds by acid anhydrides using Preyssler's anion [NaP5W30O110]14- and heteropolyacids as green catalysts

Gharib A., Jahangir M., Scheeren J.(H.)W.

Polish Journal of Chemical Technology

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2011

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Vol. 13, nr 2

11-17

EN

The Preyssler, Wells-Dowson and Keggin heteropolyacids are efficient and eco-friendly solid acid catalysts for the acylation of electron-rich aromatic compounds with acid anhydrides. The performance of different forms of heteropolyacids was compared. In all the cases, the best results were obtained using the Preyssler heteropolyacid as the catalyst. In the presence of 25 mol% (with respect to H+ equivalency) Preyssler catalyst, highly para-selective acetylation of anisole occurs using two equivalents of acetic anhydride, in 15 min at room temperature. The isolated yield of the p-methoxyacetophenone product is 98%.

3

Esters of p-Nitrophenol in Synthesis of 1-N-Monoamide and 1,7-Bis-N,N_-amide Derivatives of 1,4,7,10-Tetraazacyclododecane

Skwierawska A.

Polish Journal of Chemistry

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2006

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Vol. 80, nr 8

1353-1361

EN

The efficient synthesis of N-monoamide and bis-N,N-amide-1,4,7,10-tetraazacyclododecanes is reported.

4

Synteza nadtlenoestrów organicznych w środowisku cieczy jonowych

Chrobok A., Baj S., Siewniak A.

Chemik

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2005

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Vol. 58, nr 6

348-350

PL

W niniejszej pracy opracowano nową efektywną syntezę nadtlenoestrów organicznych w wyniku reakcji aclylowania wodoronadtlenków alkilowych wobec 30% roztworu wodnego NaOH lub pirydyny w środowisku wybranych cieczy jonowych.

EN

A new convenient and effective method of synthesis of organic peroxyesters has been developed, which involves acylation of hydroperoxides in the presence of NaOH (30% water solution) or pyridyne in room temperature ionic liquids as a novel media.

5

Effect of Base and Acyl Chloride on Regioselectivity of Acylation of 8,8-Pentamethylene-2-methyl-7,9-dioxa-1-azaspiro[4.5]dec-1-ene 1-Oxide

Koszytkowska-Stawińska M., Gębarowski P., Sas W.

Polish Journal of Chemistry

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2004

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Vol. 78 / nr 2

217-222

EN

Acylation of 2-methyl-7,9-dioxa-1-azaspiro[4.5]dec-1-ene 1-oxide (5) in the presence of pyridine gives 3-acyloxy-2-methyl-1-pyrroline derivatives 6 independently of kind of acid chloride, while treatment of 5 with benzoyl or p-nitrobenzoyl chloride and triethylamine affords mainly 2-benzoyloxymethyl- 8a and 2-p-nitrobenzoyloxymethyl-1-pyrroline 8b, respectively. Acetylation of 5 was base-independent.

6

PTC acylation of organic hydroperoxides with use of sodium carbonate as HCl scavenger: kinetic study

Baj S., Chrobok A.

Polish Journal of Applied Chemistry

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2002

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Vol. 46, nr 1

31-37

EN

The paper shows the results of the study on application of aqueous Na2CO3 solution for the reaction of alkyl hydroperoxides with acid chlorides in the presence of phase transfer (PT) catalysts. Observed reaction rate constants were determined. The effect of stirring speed, Na2CO3 amount, acid chloride structure and PT catalyst on the process run was investigated. The method has been proven to be effective, rendering high yields of peroxyesters (60-94%) under relatively mild conditions.

7

Reductive acylation of 4-nitroazoles. Synthesis of N-(4-azolyl)acetamides, N-(4-azolyl)succinimides and N-(4-azolyl)phthalimides

Suwiński J., Wagner P.

Polish Journal of Applied Chemistry

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2000

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Vol. 44, nr 1

31-35

EN

N-Azolylamides have been obtained by the reductive acylation of nitroazoles with acetic, succinic or phthalic anhydrides. N-Azolylsuccinamic and Af-azolylphthalamic acids forming from nitroazoles and the cyclic anhydrides have been cyclocondensed by the treatment with acetic anhydride - sodium acetate mixture to give respective N-azolylimides.