Reaktion #329105

Reaktionsgleichung

Intermediate 2h

8-Chloro-2-chloromethyl-3-(2-chlorophenyl)-3H-quinazolin-4-one

adenine

K2CO3

→

pale yellow solid

Ausbeute 39.0%

2-(6-Aminopurin-9-ylmethyl)-8-chloro-3-(2-chlorophenyl)-3H-quinazolin-4-one

Ausbeute 39.0%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigePrepared
2. 2
   SonstigeThe crude product was chromatographed in MeOH/CH2Cl2

Vorschrift

Prepared according to Procedure C using Intermediate 2h (100 mg, 0.294 mmol), adenine (44 mg, 0.324 mmol), K2CO3 (45 mg, 0.324 mmol), and DMF (1 mL). The crude product was chromatographed in MeOH/CH2Cl2 to provide 50 mg of a pale yellow solid (39%), mp 273.3-273.5° C. (discolors). 1H NMR (DMSO-d6) δ: 8.11 (dd, J=1.3, 8.0 Hz, 1H); 8.08 (s, 1H); 8.05 (s, 1H); 8.00 (dd, J=1.3, 7.8 Hz, 1H); 7.79-7.83 (m, 2H); 7.63-7.66 (m, 2H); 7.56 (t, J=7.9 Hz, 1H); 7.21 (br s, 2H); 5.17 (d, J=17 Hz, 1H); 4.97 (d, J=17 Hz, 1H). 13C NMR (DMSO-d6) ppm: 160.2, 156.1, 152.8, 152.2, 150.2, 143.3, 142.0, 135.6, 133.1, 132.3, 131.9, 131.1, 131.0, 130.9, 129.4, 128.4, 126.0, 122.5, 118.4, 45.0. MS (ES): m/z 438.0 (M+). Anal. calcd. for C20H13Cl2N7O.0.1CH4O.0.6H2O (0.15KCl: C, 52.09; H, 3.18; N, 21.15. Found: C, 51.85; H, 2.93; N, 21.01.

Quelle