Dimethyl Sulfide → (2-Methyl-4-nitrophenyl)methanamine
反応式
[CH3:1][C:2]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].S(C)C>O1CCCC1>[CH3:1][C:2]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:3]=1[CH2:4][NH2:5]参加物
4
反応条件
- 温度
- 70 °C
実験手順
To a stirred solution of 2-methyl-4-nitrobenzonitrile (407 mg, 2.510 mmol) in tetrahydrofuran was added 2M BH3.SMe2 in tetrahydrofuran (2.1 mL). The reaction mixture was stirred for 15 h at 70° C. The mixture was cooled to room temperature, then quenched by water. The mixture dissolved in ethyl acetate and washed with water and brine. The organic layer was dried over magnesium sulfate and filtered. The filtrate removed in vacuo. The crude was purified by column chromatography to give (2-methyl-4-nitrophenyl)methanamine (178 mg, 43%).
後処理
- temperatureThe mixture was cooled to room temperature
- customquenched by water
- dissolutionThe mixture dissolved in ethyl acetate
- washwashed with water and brine
- dry with materialThe organic layer was dried over magnesium sulfate
- filtrationfiltered
- customThe filtrate removed in vacuo
- customThe crude was purified by column chromatography
出典と根拠
- ORDレコード
- ord-6a39619e66bc49328662e870e489b077
- 出典データセット
- uspto-grants-2015_01
- 特許番号
- US08937092B2
反応ノート
読み込み中…