反応式
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[CH:4][CH:3]=1.[OH:16][C:17]1[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][C:18]=1[C:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:20].[OH-].[Na+]>C(Cl)(Cl)Cl>[ClH:1].[CH3:13][O:12][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][C:8]=1[O:14][CH3:15])[N:5]=[CH:4][CH:3]=[C:2]2[O:16][C:17]1[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][C:18]=1[C:19]([C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)=[O:20]参加物
実験手順
4-Chloro-6,7-dimethoxyquinoline (1.00 g) and 2-hydroxy-5-methylbenzophenone (1.14 g) were stirred at 170° C. for one hr. The reaction solution was cooled to room temperature. Chloroform was then added to the reaction solution, and separation was carried out with a 10% aqueous sodium hydroxide solution. The organic layer was washed with a saturated aqueous sodium hydrogencarbonate solution and saturated brine and was dried over anhydrous magnesium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by column chromatography on silica gel using hexane-acetone. Thereafter, 10% hydrochloric acid-methanol (10 ml) was added to the product, followed by concentration. The concentrate was suspended in ether, and the suspension was filtered to give the title compound (234 mg, yield 12%).
後処理
- washThe organic layer was washed with a saturated aqueous sodium hydrogencarbonate solution and saturated brine
- dry with materialwas dried over anhydrous magnesium sulfate
- customThe solvent was removed
- distillationby distillation under the reduced pressure
- customthe residue was purified by column chromatography on silica gel
- additionThereafter, 10% hydrochloric acid-methanol (10 ml) was added to the product
- concentrationfollowed by concentration
- filtrationthe suspension was filtered
出典と根拠
- ORDレコード
- ord-d9fec07b4a73464c9efe7ffbfcbddea2
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07560558B2
関連ノート
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