[F:1][C:2]1[CH:3]=[C:4]([CH:18]=[CH:19][CH:20]=1)[CH2:5][O:6][C:7]1[CH:16]=[C:15]2[C:10]([C:11](=[O:17])[NH:12][CH:13]=[N:14]2)=[CH:9][CH:8]=1.[Na].FC1C=C(C=CC=1)CO.FC1C=C2[C:35]([C:36](=[O:42])[NH:37]C=N2)=CC=1.Cl>O>[F:1][C:2]1[CH:3]=[C:4]([CH:18]=[CH:19][CH:20]=1)[CH2:5][O:6][C:7]1[CH:16]=[C:15]2[C:10]([C:11](=[O:17])[N:12]([CH2:35][C:36]([NH2:37])=[O:42])[CH:13]=[N:14]2)=[CH:9][CH:8]=17-(3-Fluoro-benzyloxy)-3H-quinazolin-4-one: Sodium (1.8 g, 78.6 mmol) was added portionwise to 3-fluorobenzyl alcohol and the resulting mixture heated at 80–90° C. for 4 h under Argon. The resulting suspension was cooled to rt and 7-fluoro-3H-quinazolin-4-one (3.2 g, 19.5 mmol) was added and the resulting mixture heated at 130–140° C. for 14 h. The solid formed was then dissolved with water (400 mL) and the mixture acidified to pH 3–4 with HCl (4 N). The resulting precipitate was then filtered off, washed with water (100 mL) and diethylether (100 mL). Recrystallisation from tetrahydrofuran: ethylacetate (1:1) afforded the title compound (3.2 g, 61%) as white crystals. MS: m/e=271.3 (M+H+).
Wird geladen…
