反应详情

温度

140 °C

N1,N1,N2-trimethylethane-1,2-diamine (0.189 mL, 1.49 mmol) was added to a suspension 5-chloro-N-(4-fluoro-2-methoxy-5-nitrophenyl)-4-(1-methylindol-3-yl)pyrimidin-2-amine (Intermediate 87, 700 mg, 1.24 mmol) and DIPEA (0.431 mL, 2.48 mmol) in DMA (5 mL). The mixture was then heated in a microwave at 140° C. for 0.5 h. The mixture was diluted with CH3OH and absorbed onto an SCX column. The column was washed with CH3OH and eluted with ˜1M methanolic ammonia. Appropriate fractions were concentrated and further purification by FCC, eluting with 0-5% methanolic ammonia in CH2Cl2 gave the title compound (561 mg, 89%) as an orange oil; 1H NMR: (CDCl3) 2.26 (6H, s), 2.53-2.58 (2H, m), 2.88 (3H, s), 3.24-3.28 (2H, m), 3.91 (3H, s), 3.98 (3H, s), 6.68 (1H, s), 7.26-7.3 (1H, m), 7.31-7.4 (2H, m), 7.50 (1H, s), 8.23 (1H, s), 8.39 (1H, s), 8.47 (1H, d), 9.07 (1H, s); m/z: ES+ MH+ 510.27.

1. customabsorbed onto an SCX column
2. washThe column was washed with CH3OH
3. washeluted with ˜1M methanolic ammonia
4. concentrationAppropriate fractions were concentrated
5. customfurther purification by FCC
6. washeluting with 0-5% methanolic ammonia in CH2Cl2