反应详情

温度

125 °C

2(1-Methyl-1H-imidazol-4-yl)-ethylamine bis hydrochloride (0.15 g, 0.757 mmol), 2-fluoro-4-formyl-benzonitrile (0.112 g, 0.757 mmol), prepared as described in Step D, and diisopropylethylamine (0.40 mL, 2.30 mmol) were heated at 125° C. for 1 h. The reaction mixture was concentrated in vacuo, partitioned between CH2Cl2 and saturated NaHCO3 solution, the aqueous layer extracted with CH2Cl2 (2×), the organic layers combined, dried (Na2SO4), filtered and concentrated to give the title compound after chromatography on SiO2 eluting with 0-3% NH4OH/CH3CN.

1. concentrationThe reaction mixture was concentrated in vacuo
2. custompartitioned between CH2Cl2 and saturated NaHCO3 solution
3. extractionthe aqueous layer extracted with CH2Cl2 (2×)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated