4-Fluorobenzyl chloride → (r)-1-(4-Fluorobenzyl)-3-methylpiperazine
反応式
[CH3:1][C@@H:2]1[CH2:7][NH:6][CH2:5][CH2:4][NH:3]1.[F:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13]Cl)=[CH:11][CH:10]=1.C(=O)([O-])O.[Na+]>C(O)C>[F:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13][N:6]2[CH2:5][CH2:4][NH:3][C@H:2]([CH3:1])[CH2:7]2)=[CH:11][CH:10]=1参加物
5
実験手順
To a solution of (2R)-2-methyl-piperizine (4.5 g, 45 mmol) in ethanol (80 mL) was added 4-fluorobenzyl chloride (5.38 mL, 45.0 mmol) and sodium hydrogen carbonate (11.3 g, 135 mmol). The reaction was refluxed overnight, cooled and concentrated. The remaining residue was diluted with dichloromethane and washed with water. The organic layer was separated and concentrated to give a clear oil. Chromatography on silica gel gave the title compound (5.0 g).
後処理
- temperatureThe reaction was refluxed overnight
- temperaturecooled
- concentrationconcentrated
- additionThe remaining residue was diluted with dichloromethane
- washwashed with water
- customThe organic layer was separated
- concentrationconcentrated
- customto give a clear oil
出典と根拠
- ORDレコード
- ord-47c853a443844d0ebba44d6152144a8d
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07098212B2
反応ノート
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