Chitosan is substance that is very widely used in the pharmaceutical and food industries, medicine and other areas. This polysaccharide has immense significance in human metabolism. It is able to affect the levels of cholesterol and lipids. Chemical modification of this polysaccharide allows the support of these attributes. A main goal is to prepare a group of amide derivatives of carboxymethyl chitosan to obtain a new group of polysaccharide derivatives and increase the benefits and attributes. The aim of carboxymethylation and subsequent two-step amidation is to achieve a high degree of substitution in the prepared derivatives. The amidation consisted methyl esterification followed by amino-de-alkoxylation with amidation reagents (nalkylamines, hydrazine and hydroxylamine). The purity and substitution degree of the prepared derivatives were monitored by vibration spectroscopic methods (FTIR and FT Raman) and organic elemental analysis.