反応式
[C:1]12([CH2:11][CH2:12][N:13]([CH2:26][CH2:27][NH:28][CH3:29])[C:14]([NH:16][CH2:17][CH2:18][CH2:19][C:20]3[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=3)=[O:15])[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].[CH3:38][O:39][CH2:40][CH2:41]Cl>O.C(OCC)C.CN(C)C=O>[C:1]12([CH2:11][CH2:12][N:13]([CH2:26][CH2:27][N:28]([CH2:41][CH2:40][O:39][CH3:38])[CH3:29])[C:14]([NH:16][CH2:17][CH2:18][CH2:19][C:20]3[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=3)=[O:15])[CH2:8][CH:7]3[CH2:6][CH:5]([CH2:4][CH:3]([CH2:9]3)[CH2:2]1)[CH2:10]2参加物
反応物 4
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 80 °C
実験手順
To N,N-dimethylformamide (20 ml) were added 1-[2-(1-adamantyl)ethyl]-1-(2-methylaminoethyl)-3-[3-(4-pyridyl)propyl]urea (1.50 g, 3.76 mmol), which was a free base of Compound No. 3-1, potassium carbonate (1.56 g, 11.3 mmol) and sodium iodide (1.69 g, 11.3 mmol) at room temperature, then 2-chloroethyl methyl ether (412 μl, 4.51 mmol) was added to the mixture, and the whole was heated at 80° C. The whole was stirred overnight, diethyl ether (50 ml) and water (100 ml) were added to the reaction mixture, and the whole was extracted. The obtained organic layer was washed with water (100 ml) and a saturated aqueous sodium chloride solution (50 ml), dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 552 mg (32.1%) of the titled compound as a pale yellow oily matter.
後処理
- extractionthe whole was extracted
- washThe obtained organic layer was washed with water (100 ml)
- dry with materiala saturated aqueous sodium chloride solution (50 ml), dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-beb3fd4514fb43ec9f20a3ae1ab5419e
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07098226B2
関連ノート
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