These common heterocyclic compound, 40497-11-8, name is Ethyl 2,3-dicyanopropanoate, 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. Computed Properties of C7H8N2O2
Add 0.01 mol of 3-fluoroaniline and a small amount of ethanol to a 250 mL round bottom three-necked flask.Under ice bath, 3.0 mL (0.035 mol) of concentrated hydrochloric acid was added dropwise with stirring.Dissolve 0.018 mol of sodium nitrite in 10 mL of water.Slowly drip into the flask, and after the completion of the dropwise addition, the reaction was carried out for 0.5 h to obtain a yellow diazonium salt solution.Add 0.01 mol of ethyl 2,3-dicyanopropionate to a three-necked flask.The prepared diazonium salt solution was dropped into the flask, and the reaction was added dropwise for 2 hours.Ammonia water was added, the pH was adjusted to 9-10, and the reaction was carried out for 2 h at room temperature.After the reaction was completed, it was extracted with 40 mL of dichloromethane, and the organic layer was washed with water (2¡Á30 mL).Wash with saturated sodium chloride solution (1¡Á40 mL), dry over anhydrous magnesium sulfate.The solvent was crystallized under reduced pressure to give the product 1.18 g,yield: 58.3%,
The synthetic route of Ethyl 2,3-dicyanopropanoate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Nanjing Tech University; Wan Rong; Chen Fuli; Han Zhenyu; Fu Xiaohuan; Jiang Peng; (17 pag.)CN108203450; (2018); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts