反应详情

Dissolve 4-chloro-6-(4-fluorophenyl)-2-(2,5-dimethyl-1H-pyrrol-1-yl)pyrimidine (60.4 mg, 0.2 mmoles) and (R)-1-(3-chloro-pyridin-2-yl)-3-methyl-piperazine (42.4 mg, 0.2 mmoles) in DMA (2.0 mL) under nitrogen atmosphere. Add anhydrous powdered K2CO3 (0.4 mmoles) to this mixture and heat at 130° C. for 24 hours. Cool, dilute with water (5 mL), extract with EtOAc (3×2 mL) and dry over MgSO4. Filter and concentrate under vacuum to afford crude product and purify by flash column chromatography using 10% EtOAc/hexane to afford the title product as white amorphous solid. NMR (CDCl3) δ 1.47 (3H, d, J=1.7), 2.45 (6H, s), 3.04 (2H, m), 3.45 (1H, t), 3.84 (2H, t), 4.35 (1H, m), 4.85 (1H, bs), 5.9 (1H, s), 6.77 (1H, s), 6.89 (1H, m), 7.14 (2H, t), 7.63 (1H, d, J=2.3), 8.06 (2H, m), 8.21 (1H, m). Mass spec m/z=477.11.

1. temperatureCool
2. extractionextract with EtOAc (3×2 mL)
3. dry with materialdry over MgSO4
4. filtrationFilter
5. concentrationconcentrate under vacuum
6. customto afford crude product
7. custompurify by flash column chromatography