Synthetic Route of 769-28-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 769-28-8, name is 4,6-Dimethyl-2-oxo-1,2-dihydropyridine-3-carbonitrile, molecular formula is C8H8N2O, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
4,6-Dimethyl-2-oxo-1,2-dihydropyridine-3-carbonitrile (20.0 g, 0.135 mol) was added to a solution of EtONa prepared from Na (3.1 g,0.135 mol) and EtOH (50 ml); the mixture was stirred for30 min, and the solvent evaporated to dryness. 4-Methylphenacyl bromide (28.8 g, 0.135 mol) and dry DMF (100 ml)was added to the resulting salt. The reaction mixture was heated on water bath at 80C for 2 h, cooled to room temperature, poured into ice water, and the formedprecipitate was filtered off. The mixture of N- and-alkylated isomers obtained in this way could be separated by two methods. Method I is based on differencein solubility of these substances (isomer 4b is less solublein CHCl3 and EtOAc than isomer 4). To separate theisomers, the obtained precipitate was placed on a Schott filter and washed with CHCl3-EtOAc, 1:1, several times.The substance remaining on the filter was recrystallized from EtOH. Method II involves the use of colum nchromatography (gradient eluting through SiO2, eluent CHCl3 followed by EtOAc).
According to the analysis of related databases, 769-28-8, the application of this compound in the production field has become more and more popular.
Reference:
Article; Babaev, Eugene V.; Nevskaya, Aleksandra A.; Dlynnikh, Ilya V.; Chemistry of Heterocyclic Compounds; vol. 51; 3; (2015); p. 269 – 274; Khim. Geterotsikl. Soedin.; vol. 51; 3; (2015); p. 269 – 274,6;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem