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ChemicalBook CAS DataBase List 2-Amino-5-chloro-3-nitropyridine

2-Amino-5-chloro-3-nitropyridine synthesis

5synthesis methods
-

Yield:5409-39-2 67%

Reaction Conditions:

Stage #1:5-chloro-2-pyridylamine with sulfuric acid;nitric acid at 55; for 1.25 h;
Stage #2: with sodium hydroxide in water; pH=11

Steps:

A40.a
To a mixture of 2-amino-5-chloropyridine (2.57 g, 20.0 mmol) and sulfuric acid (6.30 ml), huming HNO3 (0.860 ml, 21.1 mmol) was added dropwise over 15 minutes at 55 °C and stirred at 55 "C for 1 hour. After cooling, the reaction mixture was poured into ice-water (60 g) and neutralized with aqueous NaOH solution (pH = 11). The precipitated material was collected, washed with H2O and dried under reduced pressure at 50 0C to give 5-chloro-3-nitropyridin-2-amine (2.31 g, 67 %, yellow solid).

References:

SHIONOGI & CO., LTD.;EURO-CELTIQUE S.A WO2008/8398, 2008, A2 Location in patent:Page/Page column 369

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