[C:1]([NH:4][C:5]1[NH:6][C:7](=O)[C:8]2[N:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:9]=2[N:10]=1)(=[O:3])[CH3:2].CCN(C(C)C)C(C)C.O=P(Cl)(Cl)[Cl:28]>O1CCOCC1>[Cl:28][C:7]1[C:8]2[N:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:9]=2[N:10]=[C:5]([NH:4][C:1](=[O:3])[CH3:2])[N:6]=1To a suspension of 2-acetamido-6-chloro-3H-pyrido[3,2-d]pyrimidin-4-one (2.38 g, 10 mmol) and DIEA (5.2 mL, 30 mmol) in dioxane (120 mL) was added POCl3 (2.8 mL, 30 mmol). The mixture was heated to 80° C. for 2 hours. After removal of solvent, the residue was stirred with crashed ice for 10 minutes, then extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and concentrated to dryness providing the pure title compound as a brown solid (2.01 g, yield 78%) which was characterised as follows: MS (m/z) 256.9 [M+H]+.
Wird geladen…
