N-HYDROXY-HEXANAMIDINE synthesis

Yield:108724-16-9 74.6%

Reaction Conditions:

with hydroxylamine hydrochloride;sodium hydrogencarbonate in isopropyl alcohol at 80 - 85;

Steps:

38

To a solution of 0.107 g (15.4 mmol) of hydroxylamine hydrochloride in 1 1 mL of isopropyl alcohol, 1 .90 g (22.64 mmol) of sodium bicarbonate was added. The resulting mixture was stirred at 25 °C to 30 °C for 10 - 15 min. 1 .0 g (10.2 mmol) of hexanenitrile was added and stirred at 80 °C to 85 °C for 3 - 4 h. After the reaction period, the reaction mixtures was cooled to 25 °C to 30 °C, filtered and washed with 2 mL of isopropyl alcohol. The filtrate was collected and distilled out completely to obtain a crude residue. The residue with chased with 5 mL of toluene, to yield the title compound.Yield: 1 .0 g (74.6 %).

References:

WO2011/104680,2011,A1 Location in patent:Page/Page column 84