Methanol → N-(2-methyl-3-nitrobenzyl)-1-ethanamine
反応式
[CH3:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4]Cl.[CH2:13]([NH2:15])[CH3:14].CO.C([O-])([O-])=O.[K+].[K+]>C1COCC1.CCOC(C)=O>[CH3:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][NH:15][CH2:13][CH3:14]参加物
7
実験手順
A mixture of 2-methyl-3-nitrobenzylchloride (0.50 g, 2.7 mmol) and ethylamine (2.76 g, 61.2 mmol) in THF (10 ml)/MeOH (5 ml) was stirred at ambiend temperature for 48 h. The solvent was reduced and the recidue was dissolved in EtOAc/aq. K2CO3 solution. The aqueous phase was extracted with EtOAc (×2). The combined organic layers were washed with brine, dried (Na2SO4), and concentrated to give the title compound 0.46 g (86%) as a yellow oil.
後処理
- extractionThe aqueous phase was extracted with EtOAc (×2)
- washThe combined organic layers were washed with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-a2bf77eea6e747bdb65d29a0e626c0aa
- 出典データセット
- uspto-grants-2006_05
- 特許番号
- US07037925B2
反応ノート
読み込み中…