Sunitinib Impurity 20 synthesis
- Product Name:Sunitinib Impurity 20
- CAS Number:879274-72-3
- Molecular formula:C8H7FN2O2
- Molecular Weight:182.15
Yield:-
Reaction Conditions:
with hydrogenchloride;hydroxylamine hydrochloride in water at 100;
Steps:
111
4-Fluoroaniline (58.2 g, 0.50 mol) was added slowly to 10% aqueous HC1solution. This suspension was added to a mixture of chloral hydrate (95 g, 0.55 mol) and sodium sulfate (0.5 kg) in 750 mL water with mechanical stirring. Hydroxylamine hydrochloride (116 g, 1.63 mol) dissolved in water (250 mL) was added, and the resulting slurry was heated at 100 °C. After this temperature was reached, the heating mantle was removed immediately, and the solution was cooled to room temperature. The formed precipitate was collected by filtration, washed with water (2x300 mL), and dried in a vacuum oven at 60 °C. Yield: 78.2 g of JV-(4-fluorophenyl)-2-hydroxyiminoacetamide as an off-white solid.
References:
WO2006/28904,2006,A1 Location in patent:Page/Page column 112-113