Acetic Acid → 1-(3-bromophenyl)-2-methylpropan-2-amine
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([NH:12]C(=O)CCl)([CH3:11])[CH3:10])[CH:5]=[CH:6][CH:7]=1.NC(N)=S.C(O)(=O)C>C(O)C>[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([NH2:12])([CH3:10])[CH3:11])[CH:5]=[CH:6][CH:7]=1参加物
5
実験手順
A solution of N-[2-(3-bromophenyl)-1,1-dimethylethyl]-2-chloroacetamide (Preparation 17) (32.0 g, 105 mmol), thiourea (9.60 g, 126 mmol) and acetic acid (50 mL) in ethanol (250 mL) was heated to reflux overnight. The reaction mixture was cooled to room temperature and filtered, the filtrate was concentrated in vacuo and basified using aqueous sodium hydroxide solution (1M, 450 mL). The product was extracted with dichloromethane (2×500 mL) and the combined organics washed with brine (50 mL), dried (sodium sulfate) and the solvent removed in vacuo to afford the title compound as a black oil (23 g).
後処理
- temperatureto reflux overnight
- filtrationfiltered
- concentrationthe filtrate was concentrated in vacuo
- extractionThe product was extracted with dichloromethane (2×500 mL)
- washthe combined organics washed with brine (50 mL)
- dry with materialdried (sodium sulfate)
- customthe solvent removed in vacuo
出典と根拠
- ORDレコード
- ord-7e88779c2a8341b19d41e88cb7330e7a
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07538141B2
反応ノート
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