Dibenzylphosphate → Phosphoric acid dibenzyl ester 4-(4-tert-butyl-phenylamino)-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-2-ylmethyl ester
反応式
Cl[CH2:2][C:3]1[N:12]=[C:11]([NH:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])=[CH:16][CH:15]=2)[C:10]2[C:5](=[CH:6][C:7]([C:24]3[C:29]([C:30]([F:33])([F:32])[F:31])=[CH:28][CH:27]=[CH:26][N:25]=3)=[CH:8][CH:9]=2)[N:4]=1.[CH2:34]([O:41][P:42]([O-:52])([O:44][CH2:45][C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1)=[O:43])[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1>C(#N)C>[C:20]([C:17]1[CH:18]=[CH:19][C:14]([NH:13][C:11]2[C:10]3[C:5](=[CH:6][C:7]([C:24]4[C:29]([C:30]([F:32])([F:31])[F:33])=[CH:28][CH:27]=[CH:26][N:25]=4)=[CH:8][CH:9]=3)[N:4]=[C:3]([CH2:2][O:43][P:42](=[O:52])([O:44][CH2:45][C:46]3[CH:47]=[CH:48][CH:49]=[CH:50][CH:51]=3)[O:41][CH2:34][C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)[N:12]=2)=[CH:15][CH:16]=1)([CH3:23])([CH3:22])[CH3:21]参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
Heat a solution of [2-chloromethyl-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-4-yl]-(4-t-butyl-phenyl)-amine (417 mg, 0.89 mmol), Ag2O (308 mg, 1.33 mmol), and dibenzylphosphate (370 mg, 1.33 mmol) in acetonitrile at 70° C. for 18 hours. Dilute with additional acetonitrile and filter the hot solution through celite. Concentrate under reduced pressure to give a foam. Crystallize the crude product by dissolving in ether and slowly adding hexanes. Cool the resulting mixture on ice and collect the resulting solid via filtration to afford pure product.