Oximes are important functional groups in organic chemistry due to their synthetic utility as protecting groups for carbonyl groups and their ability to form other functionalities, 1�4 and their biological activity. 5 Oximes are commonly prepared by condensing aldehydes and ketones with hydroxylamines. These reactions do not always go to completion and reaction times can be long, and therefore there has been interest in more convenient and efficient methods. To avoid the typical disadvantage, conversion of aldehydes and ketones to the corresponding oximes was accomplished by using various catalysts such as organic acid/bases, 1,2,6 AcONa, alumina, 7 TiO2/SO4 2� , 2 silica gel, 8 Oxone®, 9 NaOH, 10 basic ionic liquid 1-butyl-3-methylimidazolium hydroxide, 11 polyoxometalates, 12 Na2SO4, 13 and CuSO4/K2CO3 14 under the solvent, the solvent-free or the microwave conditions. These are one and more drowbacks such as long reaction time, use of catalysts, inconvenients due to solid-sate reaction, low yields and limitaion of some carbonyl compounds. On the other hand, H. Sharghi, et al., 14 reported the catalysis of the stereoselectivity of CuSO4 and K2CO3 in the oximation of aldehydes and ketones under solvent-free conditions. Although this method show high selectivity, it is inconvenient for the large scale experiments and the industrial process due to the solvent-free condition. Therefore, we attempted to develop a more convenient and efficient solution method. According to the literatures, 15 treatment of potassium carbonate with methanol generates slightly the potassium methoxide, which may be useful for forming the free NH2OH from its salts. We describe the oximation of aldehyde and ketone using NH2OH·HCl/K2CO3 in methanol solvent.