2-Aminopropanol → 1-Methyl-2-(4-pyridyloxy)ethylamine
反応式
[NH2:1][CH:2]([CH3:5])[CH2:3][OH:4].[H-].[Na+].Cl.Cl[C:10]1[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=1>CN(C)C=O>[CH3:5][CH:2]([NH2:1])[CH2:3][O:4][C:10]1[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=1参加物
5
実験手順
6.2 g of 2-amino-1-propanol was added dropwise to a stirred mixture of 4.0 g of 60% sodium hydride and 50 mL of N,N-dimethylformamide at 5° C.-10° C. After the reaction mixture was stirred for 30 minutes, 12.5 g of 4-chloropyridine hydrochloride in limited amounts was added to the reaction mixture. The mixture was stirred for 20 hours at room temperature. After completion of the reaction, the solids were filtered off. The solvent in the filtrate was removed under reduced pressure. The residue was purified by column chromatography on silica gel to obtain 3.8 g of the desired product (yield: 30%). Refractive index: 1.5469.
後処理
- stirringThe mixture was stirred for 20 hours at room temperature
- customAfter completion of the reaction
- filtrationthe solids were filtered off
- customThe solvent in the filtrate was removed under reduced pressure
- customThe residue was purified by column chromatography on silica gel
出典と根拠
- ORDレコード
- ord-6d97a1bfa8604b93849d4516305a87c9
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05723469
反応ノート
読み込み中…