3-Bromobenzyl bromide → 1-(3-Bromobenzyl)piperidin-4-ol
反応式
[OH:1][CH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[Br:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][CH:16]=1)[CH2:12]Br>CN(C)C=O>[Br:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][CH:16]=1)[CH2:12][N:5]1[CH2:6][CH2:7][CH:2]([OH:1])[CH2:3][CH2:4]1参加物
4
実験手順
0.202 g (0.002 mol) of 4-hydroxypiperidine and 0.55 g (0.0022 mol) of 3-bromobenzyl bromide were dissolved in 5 ml of dimethylformamide and stirred at room temperature for 2 hrs. The solvent was distilled off and the residue was taken up in dichloromethane and washed with saturated bicarbonate solution and sodium chloride solution. The organic phase was dried over sodium sulfate and concentrated. 0.52 g (96%) 1-(3-bromo-benzyl)-piperidin-4-ol was obtained as a brown oil. MS: me/e (% basic peak)=271, 269 (C12H16BrNO+, 26, 26.6), 270, 268 (25.5, 22), 171, 169 (47, 48.3), 114 (76.6), 100 (100).
後処理
- distillationThe solvent was distilled off
- washwashed with saturated bicarbonate solution and sodium chloride solution
- dry with materialThe organic phase was dried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-e9bc74bbf57b4aff85256636a10ac1a1
- 出典データセット
- uspto-grants-1998_05
- 特許番号
- US05753679
反応ノート
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