反応式
[CH3:1][N:2]([CH2:4][CH:5]1[CH2:14][CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[C:10]([OH:15])[CH:11]=2)[CH2:6]1)[CH3:3].[H-].[Na+].[Br:18][C:19]1[CH:26]=[CH:25][C:22]([CH2:23]Br)=[CH:21][CH:20]=1.O>CN(C=O)C>[Br:18][C:19]1[CH:26]=[CH:25][C:22]([CH2:23][O:15][C:10]2[CH:11]=[C:12]3[C:7](=[CH:8][CH:9]=2)[CH2:6][CH:5]([CH2:4][N:2]([CH3:1])[CH3:3])[CH2:14][CH2:13]3)=[CH:21][CH:20]=1参加物
実験手順
2-(N,N-Dimethylamino)methyl-6-hydroxytetralin (5.0 g; obtained in Reference Example 16) was dissolved in DMF (130 ml), to which was added 60% oily sodium hydride (1.46 g) at 0° C. The reaction mixture was warmed to room temperature, and stirred for 1 hour. This was again cooled to 0° C., to which was added a DMF solution (20 ml) of 4-bromobenzyl bromide (10.0 g). The reaction mixture was stirred at room temperature for 2 hours, and water was added thereto, which was then extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, then dried, and concentrated. The residue was purified by alumina column chromatography (eluent: ethyl acetate/hexane=1/10) to obtain the entitled compound (3.4 g).
後処理
- temperatureThis was again cooled to 0° C., to which
- stirringThe reaction mixture was stirred at room temperature for 2 hours
- extractionwhich was then extracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materiala saturated aqueous sodium chloride solution, then dried
- concentrationconcentrated
- customThe residue was purified by alumina column chromatography (eluent: ethyl acetate/hexane=1/10)
出典と根拠
- ORDレコード
- ord-6e98dee0e6814b37ac858bc46a771f6a
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06310107B1
関連ノート
読み込み中…