反应详情

温度

0 °C

To a solution of 8-amino-6-(2,4-dichloro-phenyl)-3-morpholin-4-yl-imidazo[1,2-a]pyridine-7-carbonitrile (112 mg, 0.29 mmol) in THF (4 mL) was added a BH3.THF complex (1.0 M solution in THF, 1.2 mL, 1.2 mmol) followed by a 4M HCl solution in dioxane (2 drops). The reaction mixture was stirred and refluxed for 3 h, then cooled to 0° C. (ice bath) and poured into MeOH. The mixture was concentrated under vacuum, the remaining residue was dissolved in a 2M HCl solution in water, and the mixture was washed with Et2O (2×). The aqueous layer was frozen and lyophilized. The remaining residue was purified by recrystallization in a mixture of MeOH/AcOEt to yield the title compound (2HCl salt, 36 mg, 0.077 mmol, 27%). MS: 392 [M+1]+; HPLC: AtRet=1.13.

1. temperaturerefluxed for 3 h
2. concentrationThe mixture was concentrated under vacuum
3. dissolutionthe remaining residue was dissolved in a 2M HCl solution in water
4. washthe mixture was washed with Et2O (2×)
5. temperatureThe aqueous layer was frozen
6. customThe remaining residue was purified by recrystallization in a mixture of MeOH/AcOEt