反应详情

温度

110 °C

To 4,6-dichloro-2-pyrazin-2-yl-5-(2,4,6-trifluoro-phenyl)-pyrimidine (40 g, 0.112 mol) in 1-methyl-2-pyrrolidinone (40 mL) there is added (S)-2,2,2-trifluoro-1-methyl-ethylamine (31.6 g, 0.28 mol). The mixture is sealed and heated to 110° C. and stirred for 24 h. The reaction mixture is cooled to room temperature and diluted with IPA (120 mL) and water (120 mL) added slowly over 30 minutes to form a solid. The solid is filtered and washed with water (2×60 mL) to give 6-chloro-2-pyrazin-2-yl-N-[(1S)-2,2,2-trifluoro-1-methylethyl]-5-(2,4,6-trifluorophenyl)pyrimidin-4-amine in 84% yield and having a 98% HPLC purity and an enantiomeric excess of >99%. 1H NMR (DMSO-D6): 9.58 (d, 1H, J=1.1 Hz), 8.85 (m, 2H), 7.72 (d, 1H, J=8.8 Hz), 7.49 (m, 2H), 5.52 (m, 1H), 1.35 (d, 3H, J=7.0 Hz).

1. customThe mixture is sealed
2. temperatureThe reaction mixture is cooled to room temperature
3. additionadded slowly over 30 minutes
4. customto form a solid
5. filtrationThe solid is filtered
6. washwashed with water (2×60 mL)