反应详情

To a solution of 2-bromo-6-chloro-4-methylpyridine (415 mg, 2.0 mmol) in toluene (10 mL) was added 4-trifluoromethylaniline (325 mg, 2.0 mL), Pd2(dba)3 (50 mg, XANTPHOS (50 mg), and t-BuOK (350 mg). The mixture was microwaved 30 minutes at 120° C., filtered through Celite and washed with CH2Cl2 (3×). The combined organic layers were concentrated. The residue was purified by chromatography on silica gel (20-40% CH2Cl2 heptane) to give the product as a white solid (320 mg, 56%). 1H NMR (300 MHz, CDCl3) δ 7.53-7.63 (m, 2H), 7.41-7.49 (m, 2H), 6.70 (s, 1H), 6.61 (s, 2H), 2.28 (s, 3H). MS m/e 287.1 (M+H)

1. customThe mixture was microwaved 30 minutes at 120° C.
2. filtrationfiltered through Celite
3. washwashed with CH2Cl2 (3×)
4. concentrationThe combined organic layers were concentrated
5. customThe residue was purified by chromatography on silica gel (20-40% CH2Cl2 heptane)