2-(3,4-DIFLUORO-PHENYL)-N-HYDROXY-ACETAMIDINE synthesis

Yield:200504-48-9 89%

Reaction Conditions:

with hydroxyamino hydrochloride;anhydrous sodium carbonate in ethanol;water monomer at 80; for 3 h;

Steps:

Intermediate V-7; N-Hydroxy-2-phenyl-acetamidine

General procedure: Intermediate V-7; N-Hydroxy-2-phenyl-acetamidine To a solution of the commercially available phenyl-acetonitrile (1.0 g, 8.54 mmol) in ethanol (15 mL) and water (5.0 mL) were added Na₂C0₃ (1.81 g, 17.1 mmol) and hydroxylamine hydrochloride (1.19 g, 17.1 mmol). The reaction mixture was heated to 80 °C for 4 hours, poured into 50 mL water and extracted with EtOAc (150 mL). The organic phase was dried over Na₂S0₄ and concentrated under vacuo. The crude material was purified by flash chromatography (CE CVMeOH 95/5) to afford 1.16 g (90 %) of the title compound as a white solid. ES-MS m/e: 151.1 (M+H⁺).

References:

WO2015/140130,2015,A1 Location in patent:Page/Page column 143; 144