4-EthylbenzaMidoxiMe, 97% synthesis

Yield:65264-05-3 85%

Reaction Conditions:

with hydroxylamine hydrochloride;sodium hydrogencarbonate in methanol; for 5 h;Heating / reflux;

Steps:

21.1

4-ethyl-benzonitrile (2 g, 15 mmol), hydroxylamine hydrochloride (1.16 g, 17 mmol) and sodium bicarbonate (1.40 g, 17 mmol) were reacted in 30 ml of methanol under reflux for 5 hours. After removing the solvent, 50 ml of ethylacetate was added and the resulting solution was washed three times with 20 ml of water. An organic layer was dried over anhydrous magnesium sulfate and filtered off. Solvent was removed to obtain 2.1 g (12. 8 mmol, yield: 85%) of the title compound. Mass (EI) 165 (M++1)

References:

WO2005/40127,2005,A1 Location in patent:Page/Page column 79