Borane → 2-(4-Bromo-phenoxy)-propylamine
反応式
B.O1CCCC1.[Br:7][C:8]1[CH:19]=[CH:18][C:11]([O:12][CH:13]([CH3:17])[C:14]([NH2:16])=O)=[CH:10][CH:9]=1>CO>[Br:7][C:8]1[CH:19]=[CH:18][C:11]([O:12][CH:13]([CH3:17])[CH2:14][NH2:16])=[CH:10][CH:9]=1参加物
5
実験手順
A 1 M solution of borane in tetrahydrofuran (8.2 ml, 8.2 mmol) was added dropwise to 2-(4-bromo-phenoxy)-propionamide (0.2 g, 0.82 mmol) and the solution was stirred overnight at reflux then subsequently hydrolysed by slow addition of excess of methanol and refluxing for a further 2 hours. The solvent was removed under reduced pressure and aqueous ammonium chloride was added. The aqueous phase was extracted twice with ethyl acetate and the organics were combined, dried over anhydrous magnesium sulfate and concentrated in vacuo to give the desired product. Yield 0.13 g, 68%. LCMS method: 2, RT: 2.74 min; MI: 271-273 [M+1].
後処理
- temperatureat reflux
- temperaturerefluxing for a further 2 hours
- customThe solvent was removed under reduced pressure and aqueous ammonium chloride
- additionwas added
- extractionThe aqueous phase was extracted twice with ethyl acetate
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-8e88fb0ab6cf489bae071518bac2591b
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09394301B2
反応ノート
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