ONE-POT ELECTROCHEMICAL SYNTHESIS
2735
General procedure of alcohols oxidation. Electro-
lysis was performed in a membrane-free 150 mL
electrolyzer equipped with a water jacket, thermo-
performed using the equipment of Center for
Collective Usage “Nanotechnologies” of Platov South-
Russian State Polytechnic University.
2
meter, and mechanical stirrer. Anode (20 cm ) and
2
cathode (10 cm ) were made of platinum plates.
REFERENCES
Alcohol (0.04 mol), 4-acetylamino-2,2,6,6-tetra-
methylpiperidin-1-oxyl (0.004 mol, 0.85 g), and
1
. Kashparova, V.P., Kashparov, I.S., Zhukova, I.Yu.,
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10.1134/S1070363216110049
0
.004 mol of the corresponding pyridine base
dissolved in 40 mL of methylene chloride were put in
the electrolyzer. 0.06 mol (5.0 g) of NaHCO and
3
2
3
4
5
. Kelly, C.B., Lambert, K.M., Mercadante, M.A., Ovian, J.M.,
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0
.01 mol (1.7 g) of KI dissolved in 80 mL of distilled
water (рН of the aqueous phase 8.6) were then added.
2
The synthesis was performed at current density 0.05 A/cm
. Gaspa, S., Porcheddu, A., and De Luca, L., Tetrahedron
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j.tetlet.2016.06.115
(
current 1 A) and was complete after passing 6 F/mol
of electricity. After the reaction was complete, the
electrolyte was treated with concentrated solution of
sodium thiosulfate to remove excess of iodine. The
aqueous and organic layers were separated. The
aqueous layer was acidified with dilute hydrochloric
acid to pH 5 and extracted with methylene chloride
. Reddy, K.R., Venkateshwar, M., Maheswari, C.U., and
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(
2×20 mL); the organic phases were combined and
analyzed by means of gas chromato-mass spectrometry
as described elsewhere [1].
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1
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ACKNOWLEDGMENTS
7. Kashparova, V.P., Klushin, V.A., Leontyeva, D.V.,
Smirnova, N.V., Chernyshev, V.M., and Ananikov, V.P.,
Chem. Asian J., 2016, vol. 11, p. 2578. doi 10.1002/
asia.201600801
This study was financially supported by the Russian
Science Foundation (project no. 16-13-10444) and
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 87 No. 11 2017