N-HYDROXYCYCLOHEXANECARBOXIMIDAMIDE synthesis

Yield:633313-98-1 76.9%

Reaction Conditions:

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

Steps:

59

To a solution of 1 .9 g (27.4 mmol) of hydroxylamine hydrochloride in 22 mL of isopropyl alcohol, 3.3 g (40.3 mmol) of sodium bicarbonate was added. The resulting mixture was stirred at 25 °C to 30 °C for 10 - 15 min. 2.0 g (18.3 mmol) of cyclohexanecarbonitrile was added and stirred at 80 °C to 85 °C for 3 - 4 h. After the reaction period, the reaction mass was cooled to 25 °C to 30 °C, filtered and washed with 10 mL of isopropyl alcohol. The filtrate was collected and distilled out completely to obtain a crude residue. The residue was chased with 5 mL of toluene, to yield the title compound.Yield: 2.0 g (76.9 %)

References:

WO2011/104680,2011,A1 Location in patent:Page/Page column 95