6-Hydroxy-5-nitronicotinonitrile synthesis
- Product Name:6-Hydroxy-5-nitronicotinonitrile
- CAS Number:320405-84-3
- Molecular formula:C6H3N3O3
- Molecular Weight:165.11
320405-83-2
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Yield:320405-84-3 75%
Reaction Conditions:
with trichlorophosphate at 0 - 50; for 1 h;
Steps:
2 Step 2 - Synthesis of 6-hydroxy-5-nitropyridine-3-carbonitrile:
Phosphorus(V) oxychloride (0.66 mL, 7.1 mmol) was added to DMF (11 mL) at 0°C and the resulting mixture was stirred at the same temperature for 15 mm. Intermediate (aminooxy)(6-hydroxy-5-nitropyridin-3-yl)methanone (1.1 g, 6.0 mmol) was added portionwise. The reaction mixture was heated at 50°C for 1 hour then was cooled to 0°C. Water (12 mL) was added, the precipitate was collected by filtration and washed with additional water (6 mL). Acetonitrile was added to the solid and evaporated under vacuum several times toremove residual water. The obtained title compound (0.74 g, 4.5 mmol,75% yield) was progressed without any further purification. LC-MS (MH ) = 166.1
References:
WO2017/211759,2017,A1 Location in patent:Page/Page column 120
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6635-31-0
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