反応式
[Br:1][CH2:2][C:3]([CH3:8])([CH3:7])[C:4](O)=[O:5].C(Cl)(=O)C(Cl)=O.Cl.Cl.[CH3:17][C:18]1[CH:23]=[CH:22][C:21]([N:24]2[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]2)=[CH:20][CH:19]=1.CCN(C(C)C)C(C)C>C(Cl)Cl>[Br:1][CH:26]1[NH:27][CH2:28][CH2:29][N:24]([C:21]2[CH:20]=[CH:19][C:18]([CH3:17])=[CH:23][CH:22]=2)[CH2:25]1.[CH3:2][C:3]([CH3:8])([CH3:7])[CH:4]=[O:5]参加物
実験手順
3-Bromo-2,2-dimethylpropionic acid (10.0 g, 55.3 mmol) was dissolved in DCM (60 mL). Oxalyl chloride (7.20 mL, 82.9 mmol) was added slowly over 10 minutes. The reaction mixture was stirred at room temperature for 18 hours and then concentrated in vacuo. The residue was dissolved in DCM (40 mL) and added to a solution of 4-methylphenyl-piperazine dihydrochloride (13.76 g, 55.3 mmol) and DIPEA (33.0 mL, 193.4 mmol) in DCM (100 mL) at 0° C. The reaction mixture was allowed to warm to room temperature over 1 hour and then stirred at room temperature for 16 hours. The reaction mixture was washed with 10% citric acid solution (2×100 mL), dried (MgSO4) and concentrated in vacuo to give 3-bromo-1-(4-methylphenyl)piperazine-2,2-dimethylpropan-1-one (9.62 g, 52%) as a white solid which was used without further purification.
後処理
- concentrationconcentrated in vacuo
- dissolutionThe residue was dissolved in DCM (40 mL)
- temperatureto warm to room temperature over 1 hour
- stirringstirred at room temperature for 16 hours
- washThe reaction mixture was washed with 10% citric acid solution (2×100 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-43dd9f090fc14470b0593744eb01787f
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08093248B2
関連ノート
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