2-hydroxy-5-nitrobenzamide synthesis
- Product Name:2-hydroxy-5-nitrobenzamide
- CAS Number:2912-78-9
- Molecular formula:C7H6N2O4
- Molecular Weight:182.13
17302-46-4
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Yield:2912-78-9 73%
Reaction Conditions:
with ammonium hydroxide at 50; for 48 h;Inert atmosphere;
Steps:
1 2-Hydroxy-5-nitrobenzamide
Methyl 5-nitrosalicylate (4.0g, 20.29mmol) was added to the ammonia water (70mL) solution, nitrogen protection reaction system, heated to 50 °C stirred reaction for 2 days. After the end of the reaction, the reaction liquid was distilled dry by reducing pressure, pure water (30mL) was added to the residue, and the hydrochloric acid solution was adjusted to near acidity with 2mol/L hydrochloric acid solution. Ethyl acetate extract (3×50mL), combined with anhydrous sodium sulfate in the organic layer dried for 2-3 hours, filtered and concentrated, silica gel column chromatography (petroleum ether / ethyl acetate = 30%-50%), to give a yellowish solid (2.70g, 73%).
References:
WO2022/160138,2022,A1 Location in patent:Page/Page column 8-9
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