反应详情

rac-Ethyl 7-(7-methoxy-2,3-dip-tolyl-7,8-dihydropyrido[2,3-b]pyrazin-5(6H)-yl)heptanoate (step 1) (139 mg, 0.277 mmol) in MeOH (3 ml) at RT was treated with 2M NaOH (416 μL, 0.831 mmol) and the mixture was stirred at RT for 4 hours. A further portion of 2M NaOH (416 μL, 0.831 mmol) was added the reaction mixture was stirred at RT overnight. The organic solvent was removed in vacuo and the resulting aqueous portion was diluted with water (20 ml). The pH was adjusted to pH1 using 2M HCl and the mixture was extracted with DCM (×3). The combined organic extracts were isolated using a phase separating cartridge and the solvent was removed in vacuo. Purification of the crude product by chromatography on silica eluting with 0-30% EtOAc/iso-hexane followed by 10% MeOH in EtOAc afforded the title compound;

1. stirringwas stirred at RT overnight
2. customThe organic solvent was removed in vacuo
3. additionthe resulting aqueous portion was diluted with water (20 ml)
4. extractionthe mixture was extracted with DCM (×3)
5. customThe combined organic extracts were isolated
6. customseparating cartridge
7. customthe solvent was removed in vacuo
8. customPurification of the crude product by chromatography on silica eluting with 0-30% EtOAc/iso-hexane