反应详情

A solution of t-butyl 2-anilino-7,8-dihydropyrido[4,3-d]pyrimidine-6(5H)-carboxylate, Intermediate 7 (2.51 g, 7.69 mmol) in acetone (20 mL) was treated with 5-6 N HCl solution in i-PrOH (6 mL) and the reaction mixture was stirred at room temperature for 27 hours. The solvent was removed in vacuo and the salt was dissolved in water. The aqueous layer was washed with EtOAc and basified with 1.0 N NaOH(aq). The alkaline mixture was extracted with CH2Cl2 (2×100 mL) and the combined CH2Cl2 extracts were dried (MgSO4), filtered, and concentrated to a yellow, crystalline solid (1.25 g, 72%).

1. customThe solvent was removed in vacuo
2. dissolutionthe salt was dissolved in water
3. washThe aqueous layer was washed with EtOAc
4. extractionThe alkaline mixture was extracted with CH2Cl2 (2×100 mL)
5. dry with materialthe combined CH2Cl2 extracts were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated to a yellow, crystalline solid (1.25 g, 72%)