3-Bromobenzyl bromide → 1-(3-Bromobenzyl)piperidin-4-ol
반응식
[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]1참가 물질
4
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-e9bc74bbf57b4aff85256636a10ac1a1
- 출처 데이터셋
- uspto-grants-1998_05
- 특허 번호
- US05753679
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