反应详情

To a solution of 2,3-dip-tolyl-5,6-dihydropyrido[2,3-b]pyrazine (Example 8.2 step 1) (3.88 g, 12.38 mmol) in DCE (70 ml) was added ethyl 7-oxoheptanoate (6.40 g, 37.1 mmol) followed by sodium triacetoxyborohydride (10.4 g, 49.1 mmol). The reaction mixture was stirred for 2 days at room temperature under an atmosphere of nitrogen. The reaction mixture was diluted with water (70 ml) and extracted with EtOAc (3×70 ml). The combined organic extracts were dried over MgSO4, filtered and concentrated in vacuo. The crude product was purified by chromatography on silica eluting with EtOAc/iso-hexane, followed by further purification using reverse phase chromatography eluting with MeCN/water (0.1% TFA) to afford the title compound;

1. extractionextracted with EtOAc (3×70 ml)
2. dry with materialThe combined organic extracts were dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude product was purified by chromatography on silica eluting with EtOAc/iso-hexane
6. customfollowed by further purification
7. washeluting with MeCN/water (0.1% TFA)