1-Methylpiperazine → 6-Methoxy-7-(3-(4-methylpiperazin-1-yl)propoxy)-3-((pivaloyloxy)methyl)-3,4-dihydroquinazolin-4-one
反応式
Br[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:15]=[C:14]2[C:9]([C:10](=[O:24])[N:11]([CH2:16][O:17][C:18](=[O:23])[C:19]([CH3:22])([CH3:21])[CH3:20])[CH:12]=[N:13]2)=[CH:8][C:7]=1[O:25][CH3:26].[CH3:27][N:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1>>[CH3:27][N:28]1[CH2:33][CH2:32][N:31]([CH2:2][CH2:3][CH2:4][O:5][C:6]2[CH:15]=[C:14]3[C:9]([C:10](=[O:24])[N:11]([CH2:16][O:17][C:18](=[O:23])[C:19]([CH3:22])([CH3:21])[CH3:20])[CH:12]=[N:13]3)=[CH:8][C:7]=2[O:25][CH3:26])[CH2:30][CH2:29]1参加物
3
反応条件
- 温度
- 100 °C
実験手順
A suspension of 7-(3-bromopropoxy)-6-methoxy-3-((pivaloyloxy)methyl) -3,4-dihydroquinazolin-4-one (36.7 g, 86 mmol) in 1-methylpiperazine (370 ml) was stirred at 100° C. for 90 minutes. After removal of the volatiles under vacuum, the residue was partitioned between methylene chloride and aqueous ammonium chloride. The organic layer was separated, washed with water, brine, dried (MgSO4) and evaporated. The solid was triturated with ether, filtered, washed with ether and dried under vacuum to give 7-(3-(4-methylpiperazin-1-yl)propoxy)-6-methoxy-3-((pivaloyloxy)methyl)-3,4-dihydroquinazolin-4-one (31.9 gr, 83%).
後処理
- customAfter removal of the volatiles under vacuum
- customthe residue was partitioned between methylene chloride and aqueous ammonium chloride
- customThe organic layer was separated
- washwashed with water, brine
- dry with materialdried (MgSO4)
- customevaporated
- customThe solid was triturated with ether
- filtrationfiltered
- washwashed with ether
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-96637d845e334c469fa286d526c39481
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08492560B2
反応ノート
読み込み中…