Hydrochloric Acid → 6-(4-Amino-2-fluorophenoxy)pyrimidin-4-amine
反応式
[NH2:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([O:8][C:9]2[CH:14]=[CH:13][C:12]([NH:15]C(=O)C)=[CH:11][C:10]=2[F:19])[CH:3]=1.Cl.C([O-])([O-])=O.[Na+].[Na+]>CO>[NH2:15][C:12]1[CH:13]=[CH:14][C:9]([O:8][C:4]2[N:5]=[CH:6][N:7]=[C:2]([NH2:1])[CH:3]=2)=[C:10]([F:19])[CH:11]=1参加物
5
実験手順
A mixture of N-(4-(6-aminopyrimidin-4-yloxy)-3-fluorophenyl)acetamide (175 mg, 0.67 mmol), 1 M HCl (6 mL), and MeOH (2 mL) was heated at reflux for 3 h. The reaction mixture was cooled, made basic (pH 8) with aqueous Na2CO3 solution and extracted with EtOAc (2×25 mL). The combined extracts were dried (MgSO4) and concentrated in vacuo to give the title compound (140 mg, 96%) as a brown solid. 1H NMR (DMSO-d6) δ 8.02 (s, 1H), 6.89 (dd, 1H, J=9.0, 9.0 Hz), 6.80 (br s, 2H), 6.43 (dd, 1H, J=12.7, 2.8 Hz), 6.35 (dd, 1H, J=8.8, 2.2 Hz), 5.67 (s, 1H), 5.34 (br s, 2H).