反应详情

Heat a mixture of 4-chloro-6-(4-fluoro-phenyl)-2-(2-methyl-pyrrolidin-1-yl)-pyrimidine (440 mg, 1.51 mmol), 1-(3-chloro-6-methoxy-pyridin-2-yl)-3-(R)-methyl-piperazine (400 mg, 1.66 mmol), and K2CO3 (230 mg, 1.66 mmol) in DMA at 120° C. for 16 hours. Partition the mixture between EtOAc and water, dry (Na2SO4) the organic layer and concentrate under reduced pressure. Purify with flash silica gel column eluting with 10% EtOAc/hexanes. Concentrate under reduced pressure to give the title compound. 1H NMR (300 MHz, CDCl3): δ1.36 (m, 6H, 2×CH3); 1.70 (m, 1H, CH2CH2); 1.93 (m, 1H, CH2CH2); 2.06 (m, 2H, CH2CH2); 3.05 (m, 2H); 3.38 (m, 1H); 3.70 (m, 2H); 3.88 (s, 3H, OCH3); 3.90 (m, 2H); 4.35 (m, 2H); 4.70 (m, 1H); 6.232 (s, 1H); 6.30 (d, 1H, J=8.4 Hz); 7.12 (m, 2H); 7.46 (d, J=9.0 Hz, 1H); 8.00 (m, 2H).

1. temperatureHeat
2. customPartition the mixture between EtOAc and water
3. dry with materialdry (Na2SO4) the organic layer
4. concentrationconcentrate under reduced pressure
5. customPurify with flash silica gel column
6. washeluting with 10% EtOAc/hexanes
7. concentrationConcentrate under reduced pressure