Synthesis
Step 2: Synthesis of 5-amino-2-methylbenzonitrile: 2-methyl-5-nitrobenzonitrile (25.0 g, 154 mmol), 10% palladium carbon catalyst (2.5 g), ethyl acetate (150 mL) and ethanol (150 mL) were mixed. The reaction mixture was stirred under hydrogen atmosphere. Upon completion of the reaction, the catalyst was removed by filtration through a pad of diatomaceous earth followed by concentration of the filtrate to afford 5-amino-2-methylbenzenecarbonitrile (19.6 g, 96% yield), the product was a tan solid. Mass spectral analysis showed m/e = 133 (M + H). Reference: Scholz, D. et al, J. Med. Chem. 41, 1050-1059 (1998).
References
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