Acetic Acid → 8,9-dihydro-7-[(5-methyl-1H-imidazol-4-yl)methylene]pyrido[1,2-a]indol-6(7H)-one
反応式
[CH3:1][C:2]1[N:6](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:5]=[N:4][C:3]=1[CH:26]=[C:27]1[C:39](=[O:40])[N:31]2[C:32]3[C:37]([CH:38]=[C:30]2[CH2:29][CH2:28]1)=[CH:36][CH:35]=[CH:34][CH:33]=3.C(O)(=O)C>O>[CH3:1][C:2]1[NH:6][CH:5]=[N:4][C:3]=1[CH:26]=[C:27]1[C:39](=[O:40])[N:31]2[C:32]3[C:37]([CH:38]=[C:30]2[CH2:29][CH2:28]1)=[CH:36][CH:35]=[CH:34][CH:33]=3参加物
反応条件
- 温度
- 80 °C
実験手順
A mixture of 8,9-dihydro-7-[(5-methyl-1-trityl-1H-imidazol-4-yl)methylene]pyrido[1,2-a]indol-6(7H)-one (21.28 g), acetic acid (500 ml), and water (80 ml) was stirred at 80° C. for 1 hour and 10 minutes. After evaporation of the solvent, the residue was diluted with water, neutralized with aqueous sodium bicarbonate solution and 3N aqueous sodium hydroxide solution, and extracted with chloroform to give precipitates. The precipitates were collected, washed with water and chloroform, and dried to give 8,9-dihydro-7-[(5-methyl-1H-imidazol-4-yl)methylene]pyrido[1,2-a]indol-6(7H)-one (5.8 g). The chloroform layer separated was washed with water and brine, dried over anhydrous magnesium sulfate, and evaporated to 50 ml. The chloroform solution was diluted with toluene and allowed to stand at room temperature overnight. The crystals were collected and washed with toluene to give a second crop of 8,9-dihydro-7-[(5-methyl-1H-imidazol-4-yl)methylene]pyrido[1,2-a]indol-6 (7H)-one (5.2 g).
後処理
- customAfter evaporation of the solvent
- additionthe residue was diluted with water
- extractionextracted with chloroform
- customto give
- customprecipitates
- customThe precipitates were collected
- washwashed with water and chloroform
- customdried
出典と根拠
- ORDレコード
- ord-bbbff88229194d0082447190ea593e57
- 出典データセット
- uspto-grants-1994_03
- 特許番号
- US05290785
反応ノート
読み込み中…