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ChemicalBook CAS DataBase List 4-Chloro-2-hydroxy-3-nitropyridine
165547-79-5

4-Chloro-2-hydroxy-3-nitropyridine synthesis

2synthesis methods
89282-12-2 Synthesis
2,4-Dihydroxy-3-nitropyridine

89282-12-2
256 suppliers
$8.00/5g

-

Yield:-

Reaction Conditions:

with N-benzyl-N,N,N-triethylammonium chloride;trichlorophosphate in water;acetonitrile;

Steps:

68.A Part A.

Part A. 4-chloro-3-nitro-2(1H)-pyridinone: To a solution of 2,4-dihydroxy-3-nitropyridine (5.00 g, 32.03 mmol) and benzyltriethylammonium chloride (29.18 g, 128.12 mmol) in 100 mL of CH3CN was added dropwise phosphorus oxychloride (11.9 mL, 128.12 mmol). The mixture was heated at 60° C. for 1 h and refluxed for 1 h. The solvent was removed and 150 mL of iced water was added. The resulting mixture was stirred at 0° C. for 1.2 h. The precipitate was filtered and dried to give 4.48 g of yellow solid as the desired product. 1H NMR (DMSO-d6) δ 7.79-7.76 (d, 1H), 6.61-6.59 (d, 1H); MS (AP+): 216.0, (M+CH3CN+H)+.

References:

US2002/183324,2002,A1

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