反応式
[C:1]([O:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:24]=[C:23](F)[CH:22]=[C:21]3[C:16]=2[C:17](=[O:26])[NH:18][CH:19]=[N:20]3)[CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[CH3:27][N:28]1[CH2:33][CH2:32][N:31]([CH2:34][CH2:35][CH2:36][OH:37])[CH2:30][CH2:29]1.CC(C)([O-])C.[K+]>COCCOCCOC.ClCCl.O>[NH3:8].[C:1]([O:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:24]=[C:23]([O:37][CH2:36][CH2:35][CH2:34][N:31]3[CH2:30][CH2:29][N:28]([CH3:27])[CH2:33][CH2:32]3)[CH:22]=[C:21]3[C:16]=2[C:17](=[O:26])[NH:18][CH:19]=[N:20]3)[CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2]参加物
反応物 3
生成物 2
試薬・触媒・溶媒 3
実験手順
5-{[1-(2-tert-butoxyethyl)piperidin-4-yl]oxy}-7-fluoroquinazolin-4(3H)-one (5.45 mg, 1.5 mmol) in anhydrous diglyme (15 ml) was reacted with 3-(4-methylpiperazin-1-yl)propan-1-ol (474 mg, 3 mmol) in the presence of potassium tert-butoxide (11.77 g, 10 mmol) at 100° C. for 4 hours. The reaction mixture was diluted with dichloromethane (10 ml) and water (10 ml) and the pH adjusted to 7.7. The mixture was extracted several times with dichloromethane and the organic phase dried (magnesium sulphate), evaporated and the residue purified by chromatography on silica gel. Elution with dichloromethane:methanolic ammonia (9:1) yielded 5-{[1-(2-tert-butoxyethyl)piperidin-4-yl]oxy}-7-[3-(4-methylpiperazin-1-yl)propoxy]quinazolin-4(3H)-one (411 mg, 55% yield):
後処理
- extractionThe mixture was extracted several times with dichloromethane
- dry with materialthe organic phase dried (magnesium sulphate)
- customevaporated
- customthe residue purified by chromatography on silica gel
- washElution with dichloromethane
出典と根拠
- ORDレコード
- ord-dbb39fb66c83498ea7f50391fc9ea242
- 出典データセット
- uspto-grants-2008_07
- 特許番号
- US07402585B2
関連ノート
読み込み中…