反应详情

To benzyl((trans)-4-(8-methylimidazo[1,5-a]pyrazin-3-yl)cyclohexyl)methylcarbamate (3.52 g, 9.05 mmol) in N,N-dimethylformamide (35 ml) was added N-bromosuccinimide (1.611 g, 9.05 mmol) and the mixture was stirred at room temperature for four hours. The reaction was quenched with saturated aqueous sodium hydrogencarbonate and subsequently extracted three times with dichloromethane. The combined organic layers were washed with brine, dried (Na2SO4) and concentrated in vacuo. The residue was purified by column chromatography (silica gel, dichloromethane with gradient 0 to 5% of methanol) to yield benzyl ((trans)-4-(1-bromo-8-methylimidazo[1,5-a]pyrazin-3-yl)cyclohexyl)methylcarbamate (3.01 g).

1. customThe reaction was quenched with saturated aqueous sodium hydrogencarbonate
2. extractionsubsequently extracted three times with dichloromethane
3. washThe combined organic layers were washed with brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography (silica gel, dichloromethane with gradient 0 to 5% of methanol)