反应详情

A yellow solution of 2,3-di-p-tolyl-7,8-dihydropyrido[2,3-b]pyrazin-6(5H)-one ((prepared according to the preparation procedures disclosed in PCT patent application PCT/EP2011/062028, Example 12.1 step 1) (2.0 g, 6.07 mmol) and ethyl 7-bromoheptanoate (2.88 g, 12.14 mmol) in DMF (40 ml) under a nitrogen atmosphere was treated with potassium carbonate (4.20 g, 30.4 mmol) and the resulting suspension was stirred at room temperature for 23 hours. The mixture was diluted with water and extracted with EtOAc (×2). The extracts were washed with water (×2) and brine, dried (MgSO4) and evaporated under reduced pressure to afford a yellow oil. The crude material was diluted with ether (50 ml) and washed with water (2×20 ml), brine, dried (MgSO4) and concentrated under reduced pressure. Purification by chromatography on silica eluting with 0-100% EtOAc in iso-hexane afforded the titled compound;

1. customaccording to the preparation procedures
2. extractionextracted with EtOAc (×2)
3. washThe extracts were washed with water (×2) and brine
4. dry with materialdried (MgSO4)
5. customevaporated under reduced pressure
6. customto afford a yellow oil
7. washwashed with water (2×20 ml), brine
8. dry with materialdried (MgSO4)
9. concentrationconcentrated under reduced pressure
10. customPurification by chromatography on silica eluting with 0-100% EtOAc in iso-hexane