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ChemicalBook CAS DataBase List 2,6-DINITRO-3-HYDROXYPYRIDINE

2,6-DINITRO-3-HYDROXYPYRIDINE synthesis

3synthesis methods
15128-82-2 Synthesis
3-Hydroxy-2-nitropyridine

15128-82-2
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$10.00/10g

-

Yield:15128-91-3 51%

Reaction Conditions:

with HNO3;acetic anhydride at 0 - 20; for 4 h;

Steps:

51.01 Step-01: Preparation of 2,6-dinitropyridin-3-ol

To a pre-mixture solution of acetic anhydride (14 mL) and nitric acid (6.2 mL) was added a solution of 2-nitropyridin-3-ol (5 g) drop wisely at 0°C temperature. Resulting solution was stirred at 0°C for 2 h followed by stirring at room temperature for additional 2 h. After completion of the reaction (monitored by TLC), the reaction mass was quenched with ice water and extracted with dichloromethane (3 x 150 mL). The combined organic layer was dried over anhydrous sodium sulfate, evaporated under reduced pressure to obtain a crude. The crude was triturated with -pentane followed by drying under reduced pressure to afford 2,6-dinitropyridin-3-ol (3.4 g, 51%) as a yellow solid.*H NMR (400 MHz, DMSO-rf6): d 10.72 (b s, 1H), 8.53 (d, 1H), 7.89-7.85 (m, 1H).

References:

WO2022/180560,2022,A1 Location in patent:Page/Page column 126