Synthesis
A mixture of aniline and ethyl cyanoacetate was added to a 20 mL round-bottom flask followed by [PyPS]3PW12O40 catalyst (140 mg, 0.04 mmol). The reaction mixture was placed in a microwave reactor, heated to the corresponding temperature at 700 W power and stirred. The reaction process was monitored by thin layer chromatography (TLC). Upon completion of the reaction, the mixture was diluted with ethyl acetate (20 mL) and stirred continuously for 30 min. The insoluble catalyst was recovered by filtration or centrifugal separation. The filtrate is evaporated and the resulting residue is nearly pure 2-cyanoacetanilide. For further purification, recrystallization or column chromatography may be used.
References
[1] Chemistry of Heterocyclic Compounds (New York, NY, United States), 1985, vol. 21, # 8, p. 998 - 1002
[2] Khimiya Geterotsiklicheskikh Soedinenii, 1985, vol. 21, # 8, p. 1202 - 1206
[3] Tetrahedron Letters, 2015, vol. 56, # 30, p. 4527 - 4531
[4] Synthesis (Germany), 2013, vol. 45, # 1, p. 45 - 52
[5] Pharmazie, 1984, vol. 39, # 1, p. 19 - 21
