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N'-HYDROXY-2-METHOXYBENZENECARBOXIMIDAMIDE synthesis

2synthesis methods
-

Yield:771-28-8 100%

Reaction Conditions:

with hydroxylamine in ethanol;water at 20 - 55; for 40 h;

Steps:

1

Hydroxylamine (Fluka 55458; 50% in water; 11.28 ml 187.76 mmol; 5 eq.) was added to a solution of 2-methoxybenzonitrile (Alrich 231231 ; 4.59 ml 37.55 mmol; 1 eq.) in EtOH (50 ml_) and the resulting mixture was stirred at room temperature for 16 hours then at 55°C for 24 hours. The solvent was then evaporated and the resulting colourless oil was further dried under high vaccum to give a white solid. The latter was triturated in n-hexane, filtered and dried to afford the title compound (6.29 g, quantitative) as a white solid. HPLC (Method A) : Rt 0.96 min (purity 99.2%).

References:

WO2009/43890,2009,A1 Location in patent:Page/Page column 53

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