Reference of 107-91-5, A common heterocyclic compound, 107-91-5, name is 2-Cyanoacetamide, molecular formula is C3H4N2O, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
General procedure: A substituted alkyl methyl ketone or cyclic ketone (1 equiv) and ethyl formate or ethyl acetic(1 equiv) was added dropwise to absolute ether solution of sodium metal (1 equiv) for 1 h whilemaintained below 20 C. After the addition, the reaction was allowed to stir in an ice bath untilthe sodium metal had disappeared. The precipitate was filtered, washed with absolute ether anddried to give the corresponding compound which was directly used for the next step without further purification. To a solution of previous product (1 equiv), and cyanoacetamide (1.05 equiv) in water was stirred6 min at room temperature. The mixture was added dropwise piperidine acetate solution (0.3 equiv),which was prepared from piperidine (1 equiv), acetic acid (1 equiv) and water (5 equiv). The solutionwas heated to reflux for 2 h. Then, the reactor was cooled to room temperature, and adjusted to pH 4 by 4 N hydrochloric acid. The resulting solid was filtered, respectively washed with water and ether,and dried to give the corresponding compound which was purified by recrystallizing using menthol as solvent. 4,6-Dimethyl-2-oxo-1,2-dihydropyridine-3-carbonitrile (1a): 58% yield, white solid, m.p. 264-266 C(lit. [24] 294 C), 1H-NMR (DMSO-d6, 600 MHz): delta 12.31 (br, 1H), 6.16 (s, 1H), 2.30 (s, 3H), 2.22 (s, 3H).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.