Methylamine → Methyl((4-phenylphenyl)methyl)amine
反応式
[C:1]1([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:5][C:4]([CH:7]=O)=[CH:3][CH:2]=1.[CH3:15][NH2:16]>ClCCl.C(O)C>[CH3:15][NH:16][CH2:7][C:4]1[CH:5]=[CH:6][C:1]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:2][CH:3]=1参加物
4
実験手順
10 g of 4-Biphenylcarbaldehyde and 40 ml of 33% ethanolic methylamine are stirred overnight at room temperature with a 4 Å molecular sieve. The mixture is filtered and concentrated under vacuum. The residue is treated in 60 ml of ethanol with 2 g of sodium borohydride and stirred for 3 hours. The solvent is removed under vacuum, the residue partitioned between ether and water and the organic phase dried and concentrated. The pure base is obtained as an oil following chromatography on silica gel with dichloromethane/ethanol=9/1 as eluant.
後処理
- filtrationThe mixture is filtered
- concentrationconcentrated under vacuum
- additionThe residue is treated in 60 ml of ethanol with 2 g of sodium borohydride
- customThe solvent is removed under vacuum
- customthe residue partitioned between ether and water
- customthe organic phase dried
- concentrationconcentrated
- customThe pure base is obtained as an oil
出典と根拠
- ORDレコード
- ord-dc424ddcc4994c25922d140a84ad302c
- 出典データセット
- uspto-grants-1992_05
- 特許番号
- US05112851
反応ノート
読み込み中…