6-Amino-N-hydroxy-3-pyridinecarboximidamide synthesis
- Product Name:6-Amino-N-hydroxy-3-pyridinecarboximidamide
- CAS Number:468068-28-2
- Molecular formula:C6H8N4O
- Molecular Weight:152.15
4214-73-7
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468068-28-2
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329-89-5
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Yield:468068-28-2 22%
Reaction Conditions:
with hydroxylamine hydrochloride;sodium carbonate in ethanol;water; for 6 h;Heating / reflux;
Steps:
C.3
A stirred mixture of commercially available 2-amino-5-cyano-pyridine [CAS-No. 4214-73-7] (5.0 g, 42 mmol), hydroxylamine hydrochloride (17.5 g, 0.25 mol) and sodium carbonate (31.1 g, 0.29 mol) in water (95 mL) and ethanol (21 mL) was heated under reflux conditions for 6 h. The reaction mixture was poured into water (150 mL) and extracted with ethyl acetate (4×100 mL). The combined organic layers were washed with brine (150 mL), dried (MgSO4) and evaporated.The crude product was purified by column chromatography on silica gel (ethyl acetate/MeOH/NH4OH 4:1:0.5) and crystallization (ethyl acetate/MeOH/hexane) to yield 6-amino-nicotinamide (1.39 g) and the title compound (1.42 g, 22%) as an off-white solid. MS (EI) 152.1 [(M)+]; mp 300° C.
References:
US2007/232583,2007,A1 Location in patent:Page/Page column 43
468068-27-1
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468068-28-2
27 suppliers
$57.00/50mg
4214-73-7
290 suppliers
$5.00/1g
468068-28-2
27 suppliers
$57.00/50mg