反应详情

A solution of (6-chloro-2-methoxy-pyrimidin-4-yl)-[2-(3,4-difluoro-phenyl)-ethyl]-amine (1.6 g), 3-cyano-phenylboronic acid (1.5 g), Cs2CO3 (8.3 g) and tetrakis(triphenylphosphine)palladium (0) (45 mg) in water (8 mL) and DME (32 mL) is heated at 90° C. for 16 hours. The solution is poured into water and extracted with EtOAc (2×200 mL). The combined extract is dried over sodium sulfate, filtered, evaporated in vacuo and chromatographed on silica gel eluting with EtOAc to afford 3-{6-[2-(3,4-difluoro-phenyl)-ethylamino]-2-methoxy-pyrimidin-4-yl}-phenol (1.1 g). MS: 379 (M+H); 1H NMR (300 MHz, CDCl3) □8.3 (1H, s); 8.2 (1H, d, J=5.1 Hz); 7.9 (1H, d (J=5.1 Hz)); 7.6 (1H, t); 7-7.2 (4H, m); 6.4 (1H, s); 5 (1H, m); 3.95 (3H, s); 3.7 (2H, t); 3 (2H, t).

1. extractionextracted with EtOAc (2×200 mL)
2. extractionThe combined extract
3. dry with materialis dried over sodium sulfate
4. filtrationfiltered
5. customevaporated in vacuo
6. customchromatographed on silica gel eluting with EtOAc