反应详情

A solution of methyl N-{5-bromo-3-[(2-chloro-3,6-difluorobenzyl)amino]pyrazin-2-yl}-β-alaninate in HOAc was heated at reflux for 4 hrs. After volatile components were removed on rotavap, the residue was taken in to a mixture of EtOAc and aq. NaHCO3. The combined organic layers from extraction was dried, concentrated, and then purified by silica gel column chromatography (EtOAc/Hexanes 4:1) to furnish 3-bromo-5-(2-chloro-3,6-difluorobenzyl)-5,7,8,9-tetrahydro-6H-pyrazino[2,3-b][1,4]diazepin-6-one.

1. temperatureat reflux for 4 hrs
2. customAfter volatile components were removed on rotavap
3. additionthe residue was taken in to a mixture of EtOAc and aq. NaHCO3
4. extractionThe combined organic layers from extraction
5. customwas dried
6. concentrationconcentrated
7. custompurified by silica gel column chromatography (EtOAc/Hexanes 4:1)