反应详情

A solution of 1-(6-chloropyrazin-2-yl)-1H-benzimidazol-6-amine (100 mg, 0.41 mmol) and cyclopropylmethylamine (424 μL, 4.1 mmol) in ethoxyethanol (2 mL) containing DIPEA (140 μL) was heated at reflux overnight under N2. The solution was concentrated under reduced pressure and the residue dissolved in EtOAc (20 mL) and washed successively with H2O (20 mL), 1M HCl (2×20 mL), H2O (20 mL) and brine (20 mL). After drying (Na2SO4) the solvent was removed under reduced pressure and the residue chromatographed eluting with dichloromethane-methanol (9:1-94:6) to separate pure product from the lower fractions (98 mg)

1. temperaturewas heated
2. temperatureat reflux overnight under N2
3. concentrationThe solution was concentrated under reduced pressure
4. dissolutionthe residue dissolved in EtOAc (20 mL)
5. washwashed successively with H2O (20 mL), 1M HCl (2×20 mL), H2O (20 mL) and brine (20 mL)
6. dry with materialAfter drying (Na2SO4) the solvent
7. customwas removed under reduced pressure
8. customthe residue chromatographed
9. washeluting with dichloromethane-methanol (9:1-94:6)
10. customto separate pure product from the lower fractions (98 mg)