HCID 67415371, 화합물 → HCID 136383504, 화합물
반응식
Cl.C([O:9][C:10]1[CH:19]=[C:18]2[C:13]([C:14]([NH:20][C:21]3[CH:26]=[CH:25][CH:24]=[C:23]([Cl:27])[C:22]=3[F:28])=[N:15][CH:16]=[N:17]2)=[CH:12][C:11]=1[O:29][CH3:30])C1C=CC=CC=1>FC(F)(F)C(O)=O>[Cl:27][C:23]1[C:22]([F:28])=[C:21]([NH:20][C:14]2[C:13]3[C:18](=[CH:19][C:10]([OH:9])=[C:11]([O:29][CH3:30])[CH:12]=3)[N:17]=[CH:16][N:15]=2)[CH:26]=[CH:25][CH:24]=1참가 물질
3
실험 절차
A solution of 7-(benzyloxy)-N-(3-chloro-2-fluorophenyl)-6-methoxyquinazolin-4-amine hydrochloride 2 (85.45 g, 0.192 mol) in trifluoroacetic acid (300 mL) was heated at 80° C. for 1 hour. The reaction mixture was the evaporated to dryness and the residues re-dissolved in methanol (200 mL). This solution was then added dropwise to a stirred aqueous solution of saturated sodium bicarbonate (500 mL). The resulting precipitate was collected by filtration, washed with acetonitrile and dried under vacuum. The crude solids were then purified by hot (100° C.) trituration with a mixture of butanone (500 mL) and MeOH (100 mL), filtered and dried to 4-[(3-chloro-2-fluorophenyl)amino]-6-methoxyquinazolin-7-ol 3 as a cream solid (45 g, 73%); 1H NMR Spectrum: (DMSO d6): 3.98 (s, 3H), 7.10 (s, 1H), 7.25-7.30 (m, 1H), 7.40-7.50 (m, 1H), 7.50-7.60 (m, 1H), 7.80 (s, 1H), 8.30 (s, 1H), 9.55 (s, 1H), 10.32 (s, 1H); Mass Spectrum: (M+H)+ 319.98