反应详情

温度

65 °C

The title compound was prepared using the procedure described by Ishihara, M. and Togo, H. Synlett 2006, 2, 227-230 and ibid Tetrahedron 2007, 63,1474-1480. Iodine (172 mg, 0.68 mg) was dissolved in tert-butanol (20 mL) and potassium carbonate (300 mg, 2.2 mmol) was added. 2,4-Dimethoxy-5-formylpyrimidine (100 mg, 0.6 mmol, Frontier) and (rac)-2,3-Bis(4-chloro-phenyl)-butane-2,3-diamine (200 mg, 0.65 mmol) was added to the mixture. This was warmed to 65° C. for 2 h. This was cooled, diluted with ethyl ether (50 mL) and filtered through Celite. After evaporating to dryness, the residue was purified by flash column chromatography (silica gel, eluting with 2-5% methanol/methylene chloride) to give rac-5-[(4S*,5R*)-4,5-bis-(4-chloro-phenyl)-4,5-dimethyl-4,5-dihydro-1H-imidazol-2-yl]-2,4-dimethoxy-pyrimidine.

1. customThe title compound was prepared
2. temperatureThis was cooled
3. filtrationfiltered through Celite
4. customAfter evaporating to dryness
5. customthe residue was purified by flash column chromatography (silica gel, eluting with 2-5% methanol/methylene chloride)