Synthesis
Step 4: Synthesis of 3-trifluoromethyl-benzene-1,2-diamine; A suspension of 2-nitro-3-(trifluoromethyl)aniline (0.678 g, 3.2 mmol) formed with 10% palladium/carbon catalyst (0.067 g) in methanol (20 mL) was subjected to a hydrogenation reaction under a hydrogen atmosphere (using a hydrogen balloon) for 2 hours. Upon completion of the reaction, the catalyst was removed by filtration and the solvent was subsequently removed by evaporation under reduced pressure to afford 2,3-diaminobenzotrifluoride as an off-white solid (0.420 g, 73.17% yield).
References
[1] Patent: WO2010/115736, 2010, A2. Location in patent: Page/Page column 102
[2] Journal of the Chemical Society, 1952, p. 4078
[3] Patent: US2005/54626, 2005, A1. Location in patent: Page/Page column 46
[4] Patent: US2010/120778, 2010, A1. Location in patent: Page/Page column 21
[5] Journal of Medicinal Chemistry, 2010, vol. 53, # 8, p. 3296 - 3304
