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An efficient one‐pot reaction has been developed for the synthesis of 2,3‐dichloroquinoxaline derivatives 3a–n. The reaction was performed in two steps via a silica gel catalyzed tandem process from o‐phenylenediamine and oxalic acid, followed by addition of phosphorus oxychloride (POCl3). A variety of 2,3‐dichloroquinoxalines have been obtained in good to excellent overall yields. Eight known compounds 3a–3h were characterized by IR, 1H‐NMR, and mass spectroscopies. Compounds 3i–3n without spectroscopic data were characterized by IR, 1H‐NMR, 13C‐NMR, and mass spectroscopies.
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